HRID921684

反应详情

EQUATION

反应方程式

HRID 921684 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A clear solution of 3-((phenylsulfonyl)methylene)oxetane (450 mg, 1.284 mmol) in methanol (10 mL) was treated with 1-benzhydrylpiperazine (389 mg, 1.541 mmol) and stirred at 50° C. overnight, more 3-((phenylsulfonyl)methylene)oxetane (100 mg) was added, stirred at 50° C. overnight and, concentrated. The crude was purified by ISCO (40 g), eluted with ethyl acetate: hexane=0-50%, the desired fractions were concentrated to yield 1-benzhydryl-4-(3-((phenylsulfonyl)methyl)oxetan-3-yl)piperazine (670 mg) as a white solid.

WORKUP

后处理

  1. stirringstirred at 50° C. overnight
  2. concentrationconcentrated
  3. customThe crude was purified by ISCO (40 g)
  4. washeluted with ethyl acetate
  5. concentrationhexane=0-50%, the desired fractions were concentrated