反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In a stirred autoclave, 0.33 g of a catalyst prepared according to Example H1 is added to a solution of 65.5 g of allyl 2-(2-chloro-5-nitrobenzoyloxy)-2-methylpropionate in 370 g of methyl ethyl ketone, 0.2 g (0.5 mol %) of FeCl2 4H2O and 22 mg (0.1 mol %) of tetramethylammonium chloride are added in addition, and the mixture is hydrogenated for 5 hours at a temperature of 140° C. and at a hydrogen pressure of 15 bar. After cooling and flushing the stirred autoclave with nitrogen, the catalyst is filtered off and rinsed with 40 g of methyl ethyl ketone. 435.5 g are obtained of a solution having a content of 13.22% of allyl 2-(2-chloro-5-aminobenzoyloxy)-2-methylpropionate (yield: 96.8 % of theory).
WORKUP
后处理
- additionare added in addition
- temperatureAfter cooling
- customflushing the stirred autoclave with nitrogen
- filtrationthe catalyst is filtered off
- washrinsed with 40 g of methyl ethyl ketone
- custom435.5 g are obtained of a solution