HRID629925

反应详情

EQUATION

反应方程式

HRID 629925 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a stirred solution of 37-2 (0.05 g, 0.18 mmol) in dioxane (1 mL) was added triethylamine (0.10 mL, 0.72 mmol) and methanesulfonyl chloride (0.017 mL, 0.21 mmol). To this resulting mixture was added 1-methanesulfonyl-piperazine (0.09 g, 0.54 mmol) and the reaction was heated to 100° C. for 3 days. The reaction was concentrated and flash column separation using a 0-5% methanol/dichloromethane gradient gave 37-3. (0.025 g, 33%). HRMS (M+H)+: observed=424.2378, calculated=424.2377

WORKUP

后处理

  1. concentrationThe reaction was concentrated
  2. customflash column separation
  3. customgave 37-3