HRID1501997

反应详情

EQUATION

反应方程式

HRID 1501997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

6-Fluoro-2-methyl-3-(2-oxiranyl)benzonitrile (prepared as described above, 4.80 g, 27.1 mmol) and (R)-4-N—BOC-2-hydroxymethyl-piperazine (8.79 g. 40.6 mmol) were suspended in EtOH (30 mL) and heated in a microwave apparatus at 150° C. for 1 h. The reaction mixture was cooled and evaporated to dryness. The residue was purified by chromatography through a 330 g ISCO Redi-sep column eluting with ethyl acetate to 5% MeOH/ethyl acetate to yield the title compound. LC-MS: M+1=394;

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. customevaporated to dryness
  3. customThe residue was purified by chromatography through a 330 g ISCO Redi-sep column
  4. washeluting with ethyl acetate to 5% MeOH/ethyl acetate