HRID1494141

反应详情

EQUATION

反应方程式

HRID 1494141 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 2200 g of crude ethyl 8-amino-4-[3-(3-pyridyl)-propyl]-octanoate in 28.8 L of dichloromethane is added 1377 g of triethylamine. The solution is cooled to 0° and a solution of 1435 g of p-chlorophenylsulfonyl chloride in 14.3 L of dichloromethane is added over a period of 45 minutes maintaining the temperature below 5°. The reaction is allowed to slowly warm up to room temperature overnight. The reaction mixture is washed 3 times with 15 L of sodium bicarbonate and then with water, dried over sodium sulfate and evaporated to dryness to yield ethyl 8-(p-chlorophenylsulfonamido)-4-[3-(3-pyridyl)-propyl]-octanoate as an oil.

WORKUP

后处理

  1. temperatureThe solution is cooled to 0°
  2. temperaturemaintaining the temperature below 5°
  3. washThe reaction mixture is washed 3 times with 15 L of sodium bicarbonate
  4. dry with materialwith water, dried over sodium sulfate
  5. customevaporated to dryness