HRID1280730

反应详情

EQUATION

反应方程式

HRID 1280730 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

(RS)-4-[1-(Toluene-4-sulfonyl)-pyrrolidin-3-ylsulfanyl]-phenol (1.9 g, 5.44 mmol) in phenol (5.1 g, 54.4 mmol) was treated with HBr (25 ml, 48%). After 4 hours stirring at 100° C., the reaction mixture was cooled to room temperature and quenched with H2O and CH2Cl2. The aqueous phase was washed with CH2Cl2 and concentrated to provide (RS)-4-(pyrrolidin-3-ylsulfanyl)-phenol hydrobromide (1.13 g, 75%) as a brown oil, MS: m/e=196.2 (M+H+). Following the general method of example 74, the compounds of example 75 to example 77 were prepared.

WORKUP

后处理

  1. temperaturethe reaction mixture was cooled to room temperature
  2. customquenched with H2O and CH2Cl2
  3. washThe aqueous phase was washed with CH2Cl2
  4. concentrationconcentrated