HRID76230

反应详情

EQUATION

反应方程式

HRID 76230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of [9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]hydrazine (250 mg, 1.0 mmol) in 4 mL of i-PrOH were added Et3N and 3-dimethylaminoacrolein. The solution was refluxed for 3 h and then at 50° C. for 2 d. The solvent removed and the residue was purified on 25 g Biotage snap column, eluted with 0-18% EtOAc in Hex (12 CV) to give 1-[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]-1H-pyrazole (80 mg, 31% yield).

WORKUP

后处理

  1. temperatureThe solution was refluxed for 3 h
  2. customThe solvent removed
  3. customthe residue was purified on 25 g Biotage snap column
  4. washeluted with 0-18% EtOAc in Hex (12 CV)