HRID1280729

反应详情

EQUATION

反应方程式

HRID 1280729 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

(RS)-4-(1-But-3-enyl-pyrrolidine-3-sulfonyl)-phenol (100 mg, 0.355 mmol), 3-bromopyridine (62 mg, 0.39 mmol), PdCl2(dppf)2-dichloromethane complex (9.3 mg, 0.01 mmol), and K2CO3 (95 mg, 0.69 mmol) were suspended in DMF (1.5 ml). After 5 hours stirring at 80° C., the reaction mixture was cooled to room temperature and concentrated. The residue was chromatographed over silica gel (CH2Cl2/MeOH 97:3 then 19/1) to provide (RS)-4-[1-(4-pyridin-3-yl-but-3-enyl)-pyrrolidine-3-sulfonyl]-phenol (100 mg, 78%) as a light orange foam, MS: m/e=359.2 (M+H+).

WORKUP

后处理

  1. temperaturethe reaction mixture was cooled to room temperature
  2. concentrationconcentrated
  3. customThe residue was chromatographed over silica gel (CH2Cl2/MeOH 97:3