HRID1515939

反应详情

EQUATION

反应方程式

HRID 1515939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of 2-(1-(3-fluoro-phenyl)-3-methyl-but-1-enyl)-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine (2.6 g, 6.2 mmol) in ethanol (8 mL) and tetrahydrofuran (15 mL) was treated with an aqueous sodium hydroxide solution (10%, 20 mL). The reaction was stirred at 80° C. for 16 h. At this time, the reaction mixture was cooled to 25° C. and the resulting precipitate was collected by filtration. The solids were washed with petroleum ether and diethyl ether and then dried under vacuum to afford 2-(1-(3-fluoro-phenyl)-3-methyl-but-1-enyl)-1H-pyrrolo[2,3-b]pyridine (1.2 g, 69%) as a white solid: 1H NMR (300 MHz, CDCl3) δ ppm 10.50 (s, 1H), 7.89 (dd, 1H, J1=4.8 Hz, J2=1.5 Hz), 7.84 (dd, 1H, J1=5.1 Hz, J2=1.5 Hz), 7.27-7.22 (m, 2H), 6.48 (d, 1H, J=2.1 Hz), 6.03 (d, 1H, J=10.5 Hz), 2.96-2.84 (m, 1H), 1.12 (s, 3H), 1.10 (s, 3H).

WORKUP

后处理

  1. temperatureAt this time, the reaction mixture was cooled to 25° C.
  2. filtrationthe resulting precipitate was collected by filtration
  3. washThe solids were washed with petroleum ether and diethyl ether
  4. customdried under vacuum