ChemicalBook CAS DataBase List ACETIC ACID 1-CYANO-2-PROPENYL ESTER

ACETIC ACID 1-CYANO-2-PROPENYL ESTER synthesis

6synthesis methods

Product Name:ACETIC ACID 1-CYANO-2-PROPENYL ESTER
CAS Number:15667-63-7
Molecular formula:C6H7NO2
Molecular Weight:125.13

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Yield:15667-63-7 99.9%

Reaction Conditions:

with sulfuric acid;Acetate de N,N-dimethylamino-4 pyridinium at 40 - 45; under 7.50075 Torr; for 1.5 h;Pressure;Reagent/catalyst;Temperature;

Steps:

1.1-4.2 1) Esterification of acrolein cyanohydrin
Acrolein cyanohydrin is fed into the first pipeline 1 at 78.5g / min, the catalyst DMAP acetate is mixed with the liquid acetic anhydride at 0.85g / min in the second pipeline 2 at 76.5g / min,At the same time, sulfuric acid is added to the second pipeline 2 at 0.95 g / min, and the second pipeline 2 communicates with the first pipeline 1,The time from the feeding point of sulfuric acid to entering the esterification reaction tower R1 is 5min, and the four components pass through the first pipeline 1.Add to the feed port of esterification reaction tower R1, feed in the tower, feed temperature 40 ;Gaseous acetic anhydride is introduced from the bottom of the esterification reaction tower R1 at a flow rate of 14.5 g / min, and the feed temperature is 45 ° C.The reaction temperature in the esterification reaction tower R1 is 45 , the absolute pressure is 1.0KPa, and the reaction residence time is 1.5h;The online conductivity meter Y1 is installed at the two thirds of the esterification reaction tower R1 and at the bottom of the tower.The conductivity of the bottom of the tower was 321.7us / cm, which confirmed that the acrolein cyanohydrin had been completely converted. 2) Preparation of ACA products The crude ACA product from the esterification reaction tower R1 is sent to the distillation tower R2 for vacuum distillation, with a temperature of 55 ° C and an absolute pressure of 1.1 KPa;The side line of the distillation column R2 obtained an ACA product with a mass content of 99.98% at 120.36 g / min.Residual acetic anhydride is obtained at the top of the distillation tower R2. A small amount of low-boiling substances such as acetic acid is circulated from the lower section of the esterification reaction tower R1 to the esterification reaction tower R1. Based on acrolein, the mass yield of 1-cyano-2-propene acetate is 99.9%.

References:

Shandong Xinhe Cheng Amino Acid Co., Ltd.;Wang Zhixuan;Chen Cong;Du Zhenyu;Li Jianjun CN111100036, 2020, A Location in patent:Paragraph 0035-0057

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