ChemicalBook CAS DataBase List Ethyl acetimidate hydrochloride

Ethyl acetimidate hydrochloride synthesis

4synthesis methods

Product Name:Ethyl acetimidate hydrochloride
CAS Number:2208-07-3
Molecular formula:C4H10ClNO
Molecular Weight:123.58

64-17-5

75-05-8

2208-07-3

2) Example 1-2: Preparation of ethyl acetimidate hydrochloride 1.6 kg of acetonitrile and 4.3 kg of ethanol were added to the reactor and the reactor was cooled to -10°C. 3.67 kg of acetyl chloride was slowly added under stirring and the reaction mixture was kept stirred at 0°C for 12 hours. After completion of the reaction, the solvent was removed by distillation under reduced pressure at 45°C. To the residue was added 11.8 kg of tert-butyl methyl ether and stirred at room temperature for 3 hours. The precipitated solid was collected by filtration and dried under vacuum at 40 °C to give 4.58 kg ethyl acetimidate hydrochloride (yield: 95%). Product characterization data: 1H-NMR (400 MHz, DMSO-d6) δ: 11.7 (s, 2H), 4.26 (q, 2H), 2.38 (s, 3H), 1.36 (t, 3H).

64-17-5 Synthesis

64-17-5
900 suppliers
$10.00/50g

75-05-8 Synthesis

75-05-8
1067 suppliers
$10.00/10g

2208-07-3
160 suppliers
$6.00/5g

Yield:2208-07-3 97%

Reaction Conditions:

with hydrogenchloride;sulfuric acid at -10 - 35; for 8 h;

Steps:

1; 2; 3 Example
An anhydrous ethanol and acetonitrile solution with a molar ratio of 1: 1 to 1.2 was added to a 500 ml three-necked flask equipped with a thermometer and a mechanical stirring device. The temperature of the system was lowered to below 5 ° C using ice water; concentrated sulfuric acid was added dropwise to In the concentrated hydrochloric acid reaction flask, the generated hydrogen chloride gas was dried and passed into a three-necked flask after drying with concentrated sulfuric acid. The ventilation rate affected the temperature of the system, so the ventilation rate was controlled, and the temperature of the system was kept below 5 ° C during the ventilation. Hydrogen chloride gas with a molar ratio of 1: 1 to 1.05, the aeration time is 3-4 hours. After the aeration, the temperature of the system is gradually increased to 20-35 ° C for the heat preservation reaction, and the heat preservation and stirring reaction is about 0.5 to 1.5 hours.The system became turbid with salt precipitation, and the temperature increased by about 5-10 ° C.Avoid excessive temperature of the system.Hydrochloric acid precipitates in large amounts, and the raw material liquid gradually decreases to completely react to form ethyl imidate hydrochloride.Calculate the yield.

References:

Ningxia Beilite Biological Technology Co., Ltd.;Beilite Chemical Co., Ltd.;Ningxia Green Qing'an Industrial Technology Institute;Ji Yuecheng;Zhao Liming;Wang Zhongjie;Wang Hui;Su Wei;Xia Xuepeng;Wang Xintong CN110305040, 2019, A Location in patent:Paragraph 0026-0035

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75-36-5 Synthesis