Tag: M.W=100-200

Reference of 651734-54-2, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 651734-54-2, name is 2,6-Difluoro-3,5-dimethoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred slurry of 2,6-difluoro-3,5-dimethoxyaniline (1.00 g, 5.29 mmol) in 6.0 M hydrogen chloride in water (9.00 mL, 54.0 mmol), a solution of sodium nitrite (0.383 g, 5.55 mmol) in water (2 mL) was added dropwise over 15 minutes at 0 C. After another 15 minutes, the resulting orange-red slurry was added to a solution of potassium iodide (3.50 g, 21.1 mmol) in water (5 mL) in small portions at 0 C. After addition, the reaction mixture was allowed to warm to room temperature and then it was stirred for 1 hout Solid precipitated which was filtered out. The solid was washed with water and dried under vacuum to give the desired product (1.15 g, 70%). 1H NMR (400 MHz, CDCl3): delta 6.68 (t, J=8.0 Hz, 1H), 3.88 (s, 6H) ppm.

The synthetic route of 2,6-Difluoro-3,5-dimethoxyaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Incyte Corporation; Lu, Liang; He, Chunhong; Yao, Wenqing; US2014/45814; (2014); A1;,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 39021-83-5, name is 1,4-Dimethoxy-2,3-dimethylbenzene, A new synthetic method of this compound is introduced below., Safety of 1,4-Dimethoxy-2,3-dimethylbenzene

To a solution of 1,4-dimethoxy-2,3-dimethylbenzene (5 g, 30 mmol) in acetic acid (350 ml) was added bromine (1.54 ml, 30 mmol). After stirring for 10 min the mixture was quenched with aqueous bisulphate and extracted into ether (3¡Á50 ml). The organic layer was dried with magnesium sulfate and then the solvent removed under reduced pressure

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Bedford, Robin B.; Bowen, John G.; Weeks, Amanda L.; Tetrahedron; vol. 69; 22; (2013); p. 4389 – 4394;,
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Related Products of 41365-75-7, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 41365-75-7 as follows.

Compound 28: To a suspension of sodium carbonate (31 g, 0.37 mol) in water (50 ml) was added a solution of 1-amino-3,3-diethoxypropane (10.00 mL, 61.81 mmol) in DCM (50 mL) followed by cooling to 0 C. benzenesulfonyl chloride (7.65 mL, 60.0 mmol) was added at 0 C. with vigorous stirring followed by warming to 20 C. and continued stirring for 2 h after which time MTBE (150 mL) was added. Organic layer was separated, washed with 1.0 M of HCl (50 mL), saturated NaHCO3 (50 g), water (50 g), concentrated and azeotroped to dry two times with MTBE (150 mL¡Á2) to provide N-(3,3-diethoxypropyl)benzenesulfonamide, 28 (17.34 g, 60.34 mmol, 97% yield) as light yellow clear oil.

According to the analysis of related databases, 41365-75-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CARLSON, ERIC; HANSEN, HANS; HAWKINS, LYNN; ISHIZAKA, SALLY; MACKEY, MATTHEW; SCHILLER, SHAWN; OGAWA, CHIKAKO; DAVIS, HEATHER; US2015/105370; (2015); A1;,
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Synthetic Route of 126-38-5,Some common heterocyclic compound, 126-38-5, name is 1-Bromo-2,2-dimethoxypropane, molecular formula is C5H11BrO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To 4-bromopyridin-2-amine (1.08 g, 6.24 mmol)Add in H2O (20mL) solution1-bromo-2,2-dimethoxypropane (5.59 g, 30.5 mmol)And 4-methylbenzenesulfonic acid (209.4 mg, 1.216 mmol).The reaction mixture was heated to reflux and stirred for 12 hours.After the reaction,Adjust to pH=10 with a saturated aqueous solution of Na2CO3.The resulting mixture was extracted with EtOAc (100 mL¡Á3).The combined organic phases were dried over anhydrous sodium sulfate.Filter and concentrate under reduced pressure.The residue was purified by silica gel column chromatography (EtOAc /EtOAcThe title compound was obtained as a yellow solid (750 mg, yield 57%).

The synthetic route of 126-38-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Jiatuo Sciences Corporation; Xi Ning; Li Minxiong; Peng Ju; Li Xiaobo; Zhang Tao; Hu Haiyang; Chen Wuhong; Bai Changlin; Ke Donghua; Chen Peng; (217 pag.)CN109776522; (2019); A;,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 3616-56-6, name is 2,2-Diethoxy-N,N-dimethylethanamine, A new synthetic method of this compound is introduced below., Recommanded Product: 2,2-Diethoxy-N,N-dimethylethanamine

General procedure: Dimethylaminoacetaldehyde diethyl acetal (5 mmol) was added to a solution of 7 (0.5 mmol) in AcOH (5mL) at room temperature, and the mixture was heated at 100 ¡ãC. After 1 h, the mixture was gradually cooled to room temperature. The mixture was diluted with AcOEt (100 mL), washed with saturated NaHCO3 solution and brine, and dried over MgSO4. The solvent was removed, and the residue was separated by silica gel column chromatography with hexane/AcOEt (5:1) to give 3, 4 and 8.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Abe, Takumi; Ishikura, Minoru; Heterocycles; vol. 90; 1; (2015); p. 673 – 680;,
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Application of 50868-73-0,Some common heterocyclic compound, 50868-73-0, name is 2-Methoxy-6-methylaniline, molecular formula is C8H11NO, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Step A: 2-cyclopentyl-N-(2-methoxy-6-methylphenyl)acetamide 3-cyclopentylpropionyl chloride (2.24 g, 15.31 mmol) was added to a mixture of 2-methoxy-6-methylaniline (2.0 g, 14.58 mmol) and triethylamine (2.24 mL, 16.04 mmol) in DCM at 0 C. The reaction mixture was progressively warmed to room temperature and stirred overnight. Ethyl acetate (200 ml) was added to the reaction mixture which was washed twice with HCl aq., 1N (100 ml). The organic layer was dried over MgSO4 and concentrated. The oily crude product was subjected to crystallization form hexanes to yield to the title compound (3.55 g, 14.37 mmol, 99%) as white crystal.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Methoxy-6-methylaniline, its application will become more common.

Reference:
Patent; Valeant Pharmaceuticals North America; US2008/45534; (2008); A1;,
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Reference of 107622-80-0, A common heterocyclic compound, 107622-80-0, name is (4-Phenoxyphenyl)methanamine, molecular formula is C13H13NO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Production example 46 0.13 g of 2-amino-6-methoxymethylnicotinic acid, 0.20 g of 4-phenoxybenzylamine, 0.27 g of triethylamine and 0.55 g of a BOP reagent were added to 2 ml of DMF. The obtained mixture was stirred at a room temperature for 16 hours. Thereafter, water was added to the reaction mixture, and it was then extracted with ethyl acetate. The organic layer was washed with water, and it was then dried over magnesium sulfate, followed by concentration under reduced pressure. The obtained residue was subjected to silica gel column chromatography, so as to obtain 0.17 g of N-(4-phenoxyphenyl)methyl-2-amino-6-methoxymethylnicotinic acid amide (hereinafter referred to as the present compound 62).The present compound 62 [Show Image] 1H-NMR (CDCl3) delta: 3.45 (3H, s), 4.40 (2H, s), 4.57 (2H, d, J = 5.8 Hz), 6.23-6.30 (1H, br m), 6.40 (2H, br s), 6.70 (1H, d, J = 8.0 Hz), 6.98-7.02 (4H, m), 7.09-7.13 (1H, m), 7.29-7.36 (4H, m), 7.61 (1H, d, J = 8.0 Hz).

The synthetic route of 107622-80-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sumitomo Chemical Company, Limited; EP2248423; (2010); A1;,
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Adding a certain compound to certain chemical reactions, such as: 2688-84-8, name is 2-Phenoxyaniline, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 2688-84-8, Recommanded Product: 2-Phenoxyaniline

General procedure: The mixture of intermediate Bn-2 (1 eq.), PTSA*H20 (i72.5 g, 3 eq) inAcetonitrile (224 ml, 1.3 M) was cooled to 5 C. using a ice bath. NaNO2 (41 .7 g, 2 eq.) in 240 ml water was added dropwise. Afier the addition was finished, the mixture was kept at 5 C. for i hr. The resulting diazonium salt was treated slowly with KI (iOO g, 2 eq.) in 300 ml watet After the completion of the reaction, the residue was extracted with EtOAc and the combined organic layer was washed with a iO% Na2SO3(0q) and then dried over Na2504. The organic layer was concentrated under reduced pressure afier filtration. The crude mixture was purified by silica-gel column chromatography to obtain intermediate Bn.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Phenoxyaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NICHEM FINE TECHNOLOGY CO., LTD.; WU, Hui-Ling; LIAO, Liang-Di; SHIEH, Shwu-Ju; CHEN, Chi-Chung; (145 pag.)US2018/155312; (2018); A1;,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 78531-29-0, name is 1,3-Dimethoxypropan-2-amine, A new synthetic method of this compound is introduced below., Product Details of 78531-29-0

A mixture of [4-BROMO-7- (2,] 4-dichlorophenyl) -2,6-dimethylpyrrolo [1, 2- b] pyridazine (0.143 g, 0.387 mmol), 1, 3-dimethoxypropan-2-amine (0.092 g, 0.774 [MMOL),] [2′-(DICYCLOHEXYLPHOSPHINO)-N, N-DIMETHYL-L, L’-BIPHENYL-2-AMINE] (0. [011] g, 0.029 mmol), Cs2CO3 (0.176 g, 0.542 mmol) and Pd2 (dba) 3 (0.018 g, 0.02 mmol) in DME (5.0 mL) is refluxed for 24 h. After cooling to room temperature, to the mixture is added [1,] 3-dimethoxypropan-2-amine (0.092 g, 0.774 mmol), 2′- (dicyclohexylphosphino)-N, N-dimethyl-1,1′-biphenyl-2-amine (0. [011] g, 0.029 mmol) and Pd2 (dba) 3 (0.018 g, 0.02 mmol). The mixture is refluxed for another 24 h. After cooling to room temperature, the mixture is filtered and washed with EtOAc. The filtrate is concentrated in vacuo to dryness, the residue is subjected to preparative TLC (silica gel, [1/5] EtOAc/heptane) to give 0.07 g (44%) of light yellow solid as the title compound: mp [154-155 C (CH2CL2/HEPTANE) ; LH] NMR (400 MHz, CDCl3) [8] 7.57 (d, J = 2.0 Hz, [1H),] 7.41 (d, J = 8.3 Hz, [1H),] 7. [36] (d, J = 8.3, 2.0 Hz, [1H),] 6. [35] (s, [1H),] 5.65 (s, 1H), 4.88 (d, [J =] 8.4 Hz, [LH),] 3.91-3. 82 (m, 1H), 3.69-3. 66 (m, 2H), 3.61-3. 55 (m, 2H), 3.45 (s, 3H), 3.44 (s, 3H), 2.33 (s, 3H), 2.21 (s, 3H); [13C] NMR (100 MHz, CDC13) [8] 150.4, 142.4, 136.4, 134.3, 134.1, 129.6, 129.3, 126.8, 123.3, 120.6, 119.3, 95.1, 88.0, 70.9, 59.3, 51.3, 22.4, 12.3 ; IR (diffuse reflectance) 3336,2924, 1560, 1490,1372, 1330,1192, 1113,1098, 1078,1051, 961,821, 811,778 cm ; MS [(EI)] m/z 407 (M+), 409 (M+) ; HRMS (FAB) calcd for C2oH23Cl2N302+H 408.1245, found 408.1244 ; Anal. Calcd for C20 H23 C12 N3 [02 :] C, 58.83 ; H, 5.68 ; N, 10.29. Found: C, 58.90 ; H, 5.78 ; N, 10.13.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; PHARMACIA & UPJOHN COMPANY; WO2004/35586; (2004); A1;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 93919-56-3, name is (4-(Trifluoromethoxy)phenyl)methanamine, This compound has unique chemical properties. The synthetic route is as follows., Formula: C8H8F3NO

A mixture of (R) -7-hydroxy-5, 6,7, 8-tetrahydro-naphthalen-1-yl)-carbamic acid phenyl ester (147.3 mg, 0.52 mmol) and 4-trifluoromethoxy-benzylamine (99.4 mg, 0.52 mmol) in DMSO (1.5 ml) was stirred at 150 &degC for 1.5 hours. The reaction mixture was cooled to room temperature, and ethylacetate and water were added. The extracted organic layer was washed with water then brine, dried over Na2S04, filtered and concentrated under reduced pressure. The obtained residue was triturated with dichloromethane and hexane to obtain N-{(R)-7-hydroxy-5, 6,7, 8-tetrahydro- naphthalen-l-yl}-N’-(4-trifluoromethoxy-benzyl)-urea (168.0 mg, 85 % yield). ‘H NMR (DMSO-d6) 5 1.54-1. 65 (m, 1H), 1. 81-1. 92 (m, 1H), 2.25-2. 38 (m, 1H), 2.68-2. 88 (m, 3H), 3. 86-3. 98 (m, 1H), 4.32 (d, J= 6.0 Hz, 2H), 4.85 (d, J= 4.1 Hz, 1H), 6. 72 (d, J=7. 5 Hz, 1H), 6.98 (t ; J= 7.5 Hz, 1H), 7.06 (t, J= 6.0 Hz, 1H), 7.34 (d, J=8.3 Hz, 2H), 7.43 (d, J=8.7 Hz, 2H), 7. 63 (d, J=7.5 Hz, 1H), 7.5 (s, 1H). Molecular weight : 380. 36 MS (M+H): 381 In vitro activity class: A Chiral HPLC (ChiralCel AD 0.49 cm x 25 cm column, n-hexane/ethanol = 90/10, flow rate 1.5 rnL/rnin) R-isomer was detected at 17.7 minutes.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 93919-56-3.

Reference:
Patent; BAYER AKTIENGESELLSCHAFT; WO2003/95420; (2003); A1;,
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