Category: 102-52-3

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. 102-52-3, name is 1,1,3,3-Tetramethoxypropane, This compound has unique chemical properties. The synthetic route is as follows., category: ethers-buliding-blocks

EXAMPLE 53 4,5,6,7-Tetrahydropyrazolo[1,5-a]pyrimidine-3-carboxylic acid, ethyl ester A stirred mixture of 10.88 g of 5-amino-4-pyrazolecarboxylic acid, ethyl ester, 11.51 g of malonaldehyde bis(dimethyl acetal) and 100 ml of glacial acetic acid was heated at reflux for 16 hours, then worked up as described in Example 50 to give 7.8 g of pyrazolo[1,5-a]pyrimidine-3-carboxylic acid, ethyl ester.

According to the analysis of related databases, 102-52-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; American Cyanamid Company; US4847256; (1989); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 102-52-3, name is 1,1,3,3-Tetramethoxypropane, A new synthetic method of this compound is introduced below., Product Details of 102-52-3

100 g of Compound 1 was added to 96 ml of water, and 5.4 ml of hydrochloric acid and 105.6 g of liquid bromine were slowly added dropwise at 0 C, and stirred at room temperature overnight.The water was spun off at 45 C, filtered, and the solid was washed several times with PE: EA and dried to give 50 g of Intermediate 3.

The synthetic route of 102-52-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Yaoya Science And Technology (Shanghai) Co., Ltd.; Zeng Zhaosen; Liang Yonghong; (6 pag.)CN109824586; (2019); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 102-52-3, name is 1,1,3,3-Tetramethoxypropane, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H16O4

Example A4 Preparation of the Compound of Formula 70.67 grams of piperidine are condensed with 1,1,3,3-tetramethoxypropane in acetic acid, concentrated and treated with 59.72 grams of 2-ethoxyethyl cyanoacetate cyanoacetate in the presence of an organic base and a solvent. [0228] The following base/solvent combinations are used:The desired product (104) is obtained in yields of 91% (96.5 grams) as an orange powder. [0230] After silica gel column chromatography (eluent: toluene/acetone) the pure product (104) is obtained yielding dark yellow crystals. [0231] Melting point: 66-67 C.

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 102-52-3.

Reference:
Patent; Winkler, Barbara; Hueglin, Dietmar; Eichin, Kai; Ehrsam, Larissa; Marat, Xavier; Richard, Herve; Kienzle, ILona Marion; Schroeder, Ute; US2014/150380; (2014); A1;,
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Ether | (C2H5)2O – PubChem

Synthetic Route of 102-52-3, A common heterocyclic compound, 102-52-3, name is 1,1,3,3-Tetramethoxypropane, molecular formula is C7H16O4, 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 glass-made reactor (inside volume: 2L) equipped with a condenser, thermometer, gas-blowing tube and stirrer was charged with 500 g of 2-methoxy ethanol, into which 36.5 g (1.00 mol) of hydrogen chloride gas was blown at 15C in 1 hour to be dissolved therein, and then 82.0 g (0.50 mol) of malondialdehyde bisdimethylacetal(1,1,3,3-tetramethoxypropane) was added at 10C. Then, 137.0 g (1.10 mols) of 2,3-dimercapto-1-propanol was added immediately to the above mixture at the same temperature, and the resultant mixture was stirred at 25C for 12 hours. After the starting compound was confirmed to disappear by gas chromatography, the reaction mixture was added, with stirring, to 1000 g of water in 30 minutes. The resultant mixture was subjected to extraction with chloroform and washing with water, and separation to obtain an organic phase. Chloroform was distilled at 45C under a vacuum to obtain a singly yellowish, transparent liquid crude product. The crude product thus prepared was purified by silica gel column chromatography (developing solvent: using mixed solvent of toluene/ethyl acetate: 60/40), to obtain 92.4 g (0.325 mol) of the dihydroxy compound represented by the following formula, which was a lightly yellowish crystal, as Example Compound No. (2-a-2). Its yield was 65% on malondialdehyde bisdimethylacetal as the starting compound. ? 270MHz 1H-NMR delta (CDCl3); 2.18 to 2.33 (m, 2H), 3.15 to 3.38 (m, 4H), 3.42 to 3.68 (m, 4H), 3.72 to 3.88 (m, 2H), 4.47 (dq, 2H), 4.72 to 4.78 (m, 2H) ? EI-MS: 284(M)

The synthetic route of 102-52-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Mitsui Chemicals, Inc.; EP1388540; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 102-52-3, name is 1,1,3,3-Tetramethoxypropane, A new synthetic method of this compound is introduced below., SDS of cas: 102-52-3

Concentrated hydrochloric acid (14.5 ml, 87 mmol) was added dropwise to the stirred mixture of 2-iodophenylhydrazine (14 g, 60 mmol) and malondialdehyde bis(dimethyl acetal) (12 g, 72 mmol) at 0 C. After the addition completed, the reaction mixture was stirred for 2 h at room temperature, and water (20 ml) was added. Then, the reaction mixture was neutralized with NaOH solution (1 M). The solution was extracted with ethyl acetate (3 * 30 ml). The organic phases were combined, and dried over anhydrous MgSO4. After the solvent was removed under reduced pressure, red oil was obtained. Yield: 11.8 g (73%). 1H NMR: delta 6.49 (t, J = 2.1 Hz, 1H, H4 of pyrazole), 7.16 (dt, J = 2.0 Hz, J = 7.9 Hz, 1H), 7.41-7.48 (m, 2H), 7.98 (dd, J = 0.9 Hz, J = 8.0 Hz, 1H) (C6H4), 7.73 (d, J = 2.3 Hz, 1H), 7.77 (d, J = 1.4 Hz, 1H) (H3 and H5 of pyrazole) ppm. 13C NMR: delta 94.4, 106.6, 128.2, 129.0, 130.2, 131.1, 140.1, 140.8, 143.4 (C6H4 and carbons of pyrazole) ppm. HRMS-ESI (m/z): 292.9547 (Calc. for C9H7IN2Na: 292.9552, [M + Na]+, 100%).

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; Cheng, Cai-Hong; Chen, Dan-Feng; Song, Hai-Bin; Tang, Liang-Fu; Journal of Organometallic Chemistry; vol. 726; (2013); p. 1 – 8;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 102-52-3, name is 1,1,3,3-Tetramethoxypropane, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H16O4

Another exemplary study was carried out as follow: Compound J and AcOH (7.5 volumes) were charged to an appropriately sized jacketed reactor. Mixing was started and the jacket was set to maintain an internal temperature of 25 C . Tetramethoxypropane (1.01 equivalents) was charged to the reactor and the j acket was set to maintain an internal temperature of 95 C. Once at temperature, the reaction continued mixing for 1.5 hours and then an IPC sample was taken. The passing criteria for this IPC was 60 C to prevent premature precipitation. Once the target volume was reached the jacket was set to maintain an internal temperature of 50 C. A 4 M solution of NaOH was then charged to the reactor via cannula to neutralize the remaining AcOH. This typically required approximately 10 volumes of the base solution. The neutralization was monitored by pH probe. Solids began to precipitate during the course of the charge. Once neutralized, the slurry was cooled to 20 C and held at that temperature for 1 hour prior to isolation via Buchner funnel. The cake was washed twice with 2 volumes of water and once with 2 volumes of MeOH. The solids were then dried to constant weight in a vacuum oven to provide Compound H. This procedure had been performed on 110 g scale to produce a granular light brown solid.

The synthetic route of 102-52-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INFINITY PHARMACEUTICALS, INC.; CRENIER, Louis; LESCARBEAU, Andre; SHARMA, Praveen; GENOV, Daniel G.; (324 pag.)WO2017/48702; (2017); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

A common heterocyclic compound, 102-52-3, name is 1,1,3,3-Tetramethoxypropane, molecular formula is C7H16O4, 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. 102-52-3.

5-Amino-1H-pyrazole-4-carboxylic acidEthyl ester (3.0 g, 19.3 mmol)In acetic acid (40 mL) and ethanol (10 mL)1,1,3,3-Tetramethoxypropane (3.48 g, 21.4 mmol) was added,The resulting reaction was stirred at 90 C overnight,Cool to room temperature,Concentrate under reduced pressure.The resulting residue was diluted with ethyl acetate (100 mL). The resulting solution was washed with saturated aqueous sodium bicarbonate (20 mL), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (DCM / EA v / v) = 6/1) to give the title compound as a light yellow solid (3.2 g, 85%).

The synthetic route of 1,1,3,3-Tetramethoxypropane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Jiatuo Sciences Corporation; Xi Ning; (88 pag.)CN104650092; (2017); B;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem