HRID2052696

反应详情

EQUATION

反应方程式

HRID 2052696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture, under N2, of 24.6 g of 1-(2-aminophenyl)indoline hydrochloride in 225 ml of dry CH2Cl2 is treated with 20.2 g of triethylamine over 10 minutes. The mixture is cooled to 0°-5° C., and kept at that temperature while a solution of 14.1 g of benzoyl chloride and 25 ml of CH2Cl2 is added dropwise over 1.0 hour. After stirring at room temperature overnight, H2O was added and the layers are separated. The organic phase is washed further with H2O, 3 N--HCl, 3 N--NaOH, again with H2O, and dried. The solvent is removed to leave an oil which crystallizes on standing to yield 1-(2-benzamidophenyl)indoline, m.p. 73°-76° C.

WORKUP

后处理

  1. temperatureThe mixture is cooled to 0°-5° C.
  2. additionis added dropwise over 1.0 hour
  3. customthe layers are separated
  4. washThe organic phase is washed further with H2O, 3 N
  5. dry with materialHCl, 3 N--NaOH, again with H2O, and dried
  6. customThe solvent is removed
  7. customto leave an oil which
  8. customcrystallizes