HRID2417972

反应详情

EQUATION

反应方程式

HRID 2417972 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-[3-(2-chlorophenothiazin-10-yl)propyl]-1-piperazineethanol (22.5 g) was added to 186 ml of dry dichloromethane containing triethylamine (7.8 ml). The stirred solution was cooled to -10° and maintained at that temperature during the dropwise addition of a solution of 5.1 ml of mesyl chloride in 50 ml of dry dichloromethane. The ice bath was then removed and the reaction was stirred overnight at room temperature. The solution was washed with 25 ml of a 5% sodium bicarbonate solution and then dried over anhydrous potassium carbonate. The solvent was removed in vacuo (bath temperature, 25°) to yield 24.2 g of 1-[3-(2-chloro-10H-phenothiazin-10-yl)propyl]-4(2-chloroethyl)piperazine 2a as an oil.

WORKUP

后处理

  1. temperatureThe stirred solution was cooled to -10°
  2. customThe ice bath was then removed
  3. washThe solution was washed with 25 ml of a 5% sodium bicarbonate solution
  4. dry with materialdried over anhydrous potassium carbonate
  5. customThe solvent was removed in vacuo (bath temperature, 25°)