HRID978430

反应详情

EQUATION

反应方程式

HRID 978430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 10.3 g of phosgene in 45 ml of toluene, the solution of 20.3 g of ethyl 2-methylaminomethyl-4-phenylbutyrate (described in example 1) in 19 ml of toluene was added over a period of 20 minutes. The mixture was stirred at room temperature for 4 hours and evaporated to dryness. The residue was stirred for 10 minutes with 100 ml of ether, the solids were filtered, the filtrates were evaporated to dryness and the residue was distilled under high vacuum to give N-methyl-N-(2-ethoxycarbonyl-4-phenylbutyl)carbamoyl chloride, bp 179°-189°/1 mm Hg.

WORKUP

后处理

  1. customevaporated to dryness
  2. stirringThe residue was stirred for 10 minutes with 100 ml of ether
  3. filtrationthe solids were filtered
  4. customthe filtrates were evaporated to dryness
  5. distillationthe residue was distilled under high vacuum