Month: June 2021

Application of 36865-41-5, The chemical industry reduces the impact on the environment during synthesis 36865-41-5, name is 1-Bromo-3-methoxypropane, I believe this compound will play a more active role in future production and life.

To a solution of the compound of Reference Example 76-1 (94.0 mg, 0.21 mmol) in DMF (5 mL), potassium carbonate (87.0 mg, 0.63 mmol) and 1-bromo-3-methoxypropane (48.0 mg, 0.31 mmol) were added, and the mixture was stirred at room temperature overnight. A saturated aqueous solution of ammonium chloride was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous solution of ammonium chloride twice and with a saturated saline solution once, then dried over sodium sulfate and filtered, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain the title compound (105.0 mg, 96%). MS (ESI+) 522 (M+1, 100%)

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, 1-Bromo-3-methoxypropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sumitomo Dainippon Pharma Co., Ltd.; IKUMA Yohei; FUKUDA Nobuhisa; IWATA Masato; KIMURA Hidenori; SUZUKI Kuniko; EP2876105; (2015); A1;,
Ether – Wikipedia,
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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. 14869-41-1, name is 2-(2-Chloroethoxy)acetic acid, A new synthetic method of this compound is introduced below., name: 2-(2-Chloroethoxy)acetic acid

A mixture of 2-(2-chloroethoxy)acetic acid (48 mg,0.34 mmol), compound 23 (200 mg, 0.34 mmol) and N-ethoxycarbonyl-2-ethoxy-1,2-dihydroquinoline(100 mg, 0.41 mmol) in THF (4 mL) was stirred at 60 C for 4 h when TLC analysis indicated completionof reaction. The reaction mixture was concentrated in vacuum and THF (5 mL) was added to theresidue. To the stirred mixture was added NaH (40 mg, 1 mmol) in portions at room temperature. Afteraddition, the mixture was stirred at room temperature for 5 h and TLC showed reaction was complete.Then NH4Cl solution (0.2 mL, concentrated solution) was added and the mixture was concentrated invacuum.The residue was recrystallized fromn-hexane and ethyl acetate to give 24zc as a brown solid(174 mg, 76.0% yield). 1H-NMR: 11.84 (s, 1H), 10.45-10.39 (m, 1H), 8.47 (s, 3H), 8.02 (s, 2H), 7.41-7.39(m, 3H), 7.28-7.26 (m, 3H), 7.23-7.19 (m, 2H), 4.90 (m, 1H), 4.34-4.28 (qd, J = 7.2 Hz, 2H), 3.92-3.89(m, 2H), 3.68-3.59 (m, 2H), 3.40-3.38 (m, 2H), 3.17-3.07 (m, 2H), 1.33-1.30 (t, J = 7.2 Hz, 3H). ESI-MS(m/z) = 695.17 [M + Na]+

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; Wei, Qunchao; Zheng, Zhichao; Zhang, Shijun; Zheng, Xuemin; Meng, Fancui; Yuan, Jing; Xu, Yongnan; Huang, Changjiang; Molecules; vol. 23; 8; (2018);,
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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. 1579-40-4, name is Di-p-tolyl Ether, A new synthetic method of this compound is introduced below., Safety of Di-p-tolyl Ether

In einem mit Argon begasten 100 ML Reaktor werden 2 g 4, 4′-OXYBIS (toluen) (CAS Reg. Nr. 1579-40-4) [10 mmol] in 39.2 ml Acetonitril unter Zusatz von 0.8 ML Dimethylsulfoxid [11. 2 mmol] bei 75 C geloest. Zur Loesung werden 60 mg Cu (OAc) 2, 30 mg FES04-7 H20 und 10 ml Wasser beigefuegt. 10.8 g NA2S208 geloest in 30 ML Wasser werden anschliessend unter heftigem Ruehren zugetropft. Nach 45 Minuten ist die Reaktion beendet. Die organische Phase wird mit Ethylacetat erschoepfend extra- hiert. Die gebildeten Produkte werden mit Hilfe der HPLC untersucht. Die Ausbeute des Dialdehyds 4, 4′-OXYBIS (benzaldehyd) (CAS Reg. Nr. 2215-76-1) betraegt 87 mol%. Damit liegt diese Ausbeute gegenueber den Ausbeuten mit bisher bekannten Oxidationsverfahren von 30-40% wesentlich hoeher, wodurch sich die Selektivitaet des erfindungsgemaessen Verfahrens auszeichnet.

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; TEX-A-TEC AG; WO2004/43891; (2004); A1;,
Ether – Wikipedia,
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These common heterocyclic compound, 36805-97-7, name is 1,1-Di-tert-butoxy-N,N-dimethylmethanamine, 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. Recommanded Product: 1,1-Di-tert-butoxy-N,N-dimethylmethanamine

Hexadecandioic acid (40.0 g, 140 mmol) was suspended in toluene (250 ml) and the mixture was heated toreflux. N,N-Dimethylformamide di-tert-butyl acetal (76.3 g, 375 mmol) was added drop-wise over 4 hours. The mixturewas refluxed overnight. The solvent was removed in vacuo at 50 C, and the crude material was suspended in dichloromethane/ethyl acetate (500 ml, 1:1) and stirred for 15 mins. The solids were collected by filtration and triturated withdichloromethane (200 ml). The filtrated were evaporated in vacuo to give crude mono-tert-butyl hexadecandioate, 30grams. This material was suspended in dichloromethane (50 ml), cooled with ice for 10 mins, and filtered. The solventwas removed in vacuo to leave 25 gram crude mono-tert-butyl hexadecandioate, which was recrystallized from heptane(200 ml) to give mono-tert-butyl hexadecandioate, 15.9 g (33 %). Alternatively to recrystallization, the mono-ester canbe purified by silica chromatography with ethyl acetate/heptane. 1H-NMR (CDCl3) delta: 2.35 (t, 2H), 2.20 (t, 2H), 1.65-1.55(m, 4H), 1.44 (s, 9H), 1.34-1.20 (m, 20 H).

The synthetic route of 1,1-Di-tert-butoxy-N,N-dimethylmethanamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Novo Nordisk A/S; HOEG-JENSEN, Thomas; JAKOBSEN, Palle; SENSFUSS, Ulrich; FLEDELIUS, Christian; RIBEL-MADSEN, Ulla; (32 pag.)EP2448962; (2016); B1;,
Ether – Wikipedia,
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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. 437-83-2, name is 3-Fluoro-2-methoxyaniline, A new synthetic method of this compound is introduced below., SDS of cas: 437-83-2

General procedure: NaNO2 (12.0 g, 173 mmol, in 40 mL of water) solution was addeddropwise to the mixture of 3-fluoro-2-methoxyaniline (20.0 g, 158 mmol) in 200 mL of hydrobromic acid (47 %) and100 mL of water at -5 ~ 0 C and stirred for 1 hour. This solution was then added slowly to the suspension of CuBr(45.2 g, 315 mmol) in 50 mL of hydrobromic acid (47 %) at 0 C. The resulting mixture was stirred at 0 C for 1 hourthen warmed to 50 C and stirred for 1 hour. The reaction mixture was poured into ice water and extracted withether (2 X 500 mL). The combined organic layer was washed with brine, dried over anhydrous Na2SO4 and concentratedto give 1-bromo-3-fluoro-2-methoxybenzene.

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; Merck Sharp & Dohme Corp.; PASTERNAK, Alexander; BLIZZARD, Timothy; CHOBANIAN, Harry; DE JESUS, Reynalda; DING, Fa-Xiang; DONG, Shuzhi; GUDE, Candido; KIM, Dooseop; TANG, Haifeng; WALSH, Shawn; PIO, Barbara; JIANG, Jinlong; (128 pag.)EP2744499; (2016); B1;,
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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 38336-04-8 as follows. Product Details of 38336-04-8

(1) Take 10g of bromonitrobenzene dissolved inIn 50 ml acetonitrile,6.5 g 2-benzyloxyethylamine was added to the above solution under ice bath.Then add 20 ml of triethylamine,Reaction at room temperature for 6 hours,A yellow clear solution is obtained,The reaction solution was concentrated under reduced pressure,Dissolved in 200 ml of dichloromethaneWash 50 ml of water three timesCombine the organic phase,Dry with anhydrous sodium sulfateAfter filtration, spin dry to obtain a crude product.After purifying crude product column chromatography, it will be 10.8Compound II,Yield 91.7%.

According to the analysis of related databases, 38336-04-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Tierxi (Nanjing) Pharmaceutical Research And Development Co., Ltd.; Li Yantao; Mao Yu; Zhang Chi; Liu Chun; Cui Xilin; (13 pag.)CN107586291; (2018); A;,
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22236-10-8, name is 4-(Difluoromethoxy)aniline, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Application In Synthesis of 4-(Difluoromethoxy)aniline

The nitro ether (149 mmol) was dissolved in ethanol (37.5 mL), diluted with water (25 mL), and was treated with ammonium chloride (84.7 mmol) and iron powder (105 mmol). The reaction mixture was heated at reflux for 30 minutes and the suspension was filtered through Celite. The filter cake was washed with ethanol three times and the combined filtrates were concentrated. The residue was dissolved in water and the pH adjusted to 9-10 with 5 M sodium hydroxide. The aqueous layer was extracted with ethyl acetate (3×100 mL) and the combined organic layers were dried (magnesium sulfate) and concentrated to a yellow oil. The oil was dissolved in acetic anhydride (23.5 mmol) and the reaction mixture was maintained at rt for 16 h. The reaction mixture was diluted with water (50 mL) and was neutralized with solid sodium bicarbonate. The precipitated solids were isolated by filtration, washed with water, and dried to provide the acetamide in 62% yield as a light yellow solid.

The synthetic route of 22236-10-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Xie, Wenge; Herbert, Brian; Ma, Jianguo; Nguyen, Truc Minh; Schumacher, Richard; Gauss, Carla Maria; Tehim, Ashok; US2005/250808; (2005); A1;,
Ether – Wikipedia,
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Related Products of 20781-20-8, 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. 20781-20-8, name is (2,4-Dimethoxyphenyl)methanamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

According to Scheme 35, a 10 mL micro wavable vial was charged with compound 10 (250 mg, 0.73 mmol), 2,4-dimethoxybenzylamine (Aldrich, 0.54 mL, 3.63 mmol), Pd2(dba)3 (21 mg, 0.036 mmol), NaOBu-t (140 mg, 1.46 mmol), BINAP (45 mg, 0.07 mmol) and dioxane/DMF (3 mL/1 mL). The mixture was purge with argon and then stirred at 160C under microwave for 20 min. The reaction mixture was cooled to room temperature and diluted with EtOAc. The EtOAc was isolated and dried over MgS04. The EtOAc was evaporated and the residue was subjected to flash column chromatography (hexanes/EtOAc) to give compound 11 as white solid (yield 55%) (m/z + H) 474.

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, (2,4-Dimethoxyphenyl)methanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PURDUE PHARMA L.P.; NI, Chiyou; SHAO, Bin; TAFESSE, Laykea; YAO, Jiangchao; YU, Jianming; ZHOU, Xiaoming; WO2012/35421; (2012); A2;,
Ether – Wikipedia,
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Electric Literature of 10103-06-7, A common heterocyclic compound, 10103-06-7, name is 2,3-Dimethoxynaphthalene, molecular formula is C12H12O2, 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.

(a) 1-(6,7-Dimethoxy-naphthalen-2-yl)-2-methyl-propan-1-one The solution of 2,3-dimethoxynaphthalene (16.5 g), isobutyroylchloride (12.5 g) and aluminum chloride (15.7 g) in methylene chloride (200 ml) was stirred at ambient temperature overnight. The solution was then washed with saturated sodium bicarbonate and water, dried with sodium sulfate and evaporated. Finally the crude product was triturated with ether. Yield: 13.5 g, melting point 103-105 C. 1H-NMR (DMSO-d6): 8.51 (s,1H), 7.83 (s,2H), 7.53 (s,1H), 7.39 (s,1H), (s,3H), 3.91 (s,3H), 3.76-3.80 (m,1H), 1.16 (d,6H, J=8 Hz).

The synthetic route of 10103-06-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Baeckstroem, Reijo; Pystynen, Jarmo; Lotta, Timo; Ovaska, Martti; Taskinen, Jyrki; US2004/34011; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

54149-17-6, name is 1-Bromo-2-(2-methoxyethoxy)ethane, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Application In Synthesis of 1-Bromo-2-(2-methoxyethoxy)ethane

Hydrazinemonohydrate and ethanol were put into a reaction container under a nitrogen atmosphere. A compound represented by Formula 1-122-1) was added, rollowed by heating and stirring The resultant product was concentrated to obtain a mixture containing a compound represented ny Formula (i-±2/–L)

The synthetic route of 54149-17-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DIC CORPORATION; TENG, Yan; HORIGUCHI, Masahiro; KADOMOTO, Yutaka; KOISO, Akihiro; HAYASHI, Masanao; SAITOU, Yoshitaka; LI, Zhimin; (201 pag.)WO2017/79867; (2017); A1;,
Ether – Wikipedia,
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