HRID873567

反应详情

EQUATION

反应方程式

HRID 873567 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a 50 mL round-bottomed flask was added tert-butyl 4-(4-(1-(6-chloropyridazin-3-yl)azetidine-3-carboxamido)phenyl)piperidine-1-carboxylate (550 mg, 1.165 mmol) and Pd/C (93 mg, 0.087 mmol). The flask was flushed with nitrogen for 10 minutes and ethanol (11.7 ml) was added. Triethylamine (0.162 ml, 1.165 mmol) and cyclohexa-1,4-diene (654 mg, 8.16 mmol) were added and the reaction was stirred at 80° C. for 1 hour, cooled and filtered through diatomaceous earth. The filtrate was concentrated in vacuo and the residue was purified by regular phase flash column chromatography to give the title compound.

WORKUP

后处理

  1. customThe flask was flushed with nitrogen for 10 minutes
  2. additionethanol (11.7 ml) was added
  3. temperaturecooled
  4. filtrationfiltered through diatomaceous earth
  5. concentrationThe filtrate was concentrated in vacuo
  6. customthe residue was purified by regular phase flash column chromatography