HRID1408957

反应详情

EQUATION

反应方程式

HRID 1408957 的结构方程式

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of Preparation 5 (41.8 mg, 0.152 mmol) and (±)-(1S,2S)-2-amino-1-methylcyclohexanol hydrobromide (32 mg, 0.152 mmol) in DMF (0.4 mL) was added DIPEA (0.08 mL, 0.46 mmol) and the mixture was heated to 90° C. for 18 h. The reaction was cooled to rt and added water (3 mL) then stirred rapidly for 3 h and filtered. The solids were purified on silica gel (100% heptane to 50% ethyl acetate/heptane to 100% ethyl acetate) to afford the title compound (31.6 mg, 57% yield). LCMS 369.05 (M+2)+.

WORKUP

后处理

  1. temperatureThe reaction was cooled to rt
  2. filtrationfiltered
  3. customThe solids were purified on silica gel (100% heptane to 50% ethyl acetate/heptane to 100% ethyl acetate)