HRID131448

反应详情

EQUATION

反应方程式

HRID 131448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Combine 7-fluoro-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulen-10-ylamine hydrochloride (270 mg, 0.95 mmol), (S)-2-(3-methoxy-propyl)-piperazine (330 mg, 2 mmol) in a mixture of toluene and dimethylsulfoxide (1:2) and stir at 110° C. for 24 hours. Evaporate the mixture then purify by flash chromatography, eluting with a step gradient starting with dichloromethane going to 5% 2N ammonia-methanol in dichloromethane gives (S)-7-fluoro-10-[3-(3-methoxy-propyl)-piperazin-1-yl]-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulene (320 mg, 0.82 mmol): mass spectrum (APCI): m/z=389.1 (M+1).

WORKUP

后处理

  1. customEvaporate the mixture
  2. customthen purify by flash chromatography
  3. washeluting with a step gradient