HRID1962814

反应详情

EQUATION

反应方程式

HRID 1962814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-(1H-pyrazol-4-yl)-7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]-pyrimidine (61.4 mg, 0.195 mmol) and 1-[(E)-2-cyanovinyl]cyclopropanecarbonitrile (23 mg, 0.19 mmol) in ACN (2 mL) was added DBU (58 μL, 0.39 mmol) and the resulting mixture was stirred for 16 hours. The ACN was evaporated, and the residue was dissolved in ethyl acetate. This solution was washed with 1.0 N HCl, water, and brine, and dried over sodium sulfate, and the solvent removed in vacuo. Flash column chromatography (eluting with a gradient from 0-80% ethyl acetate in hexanes) afforded the product (49 mg, 58%).

WORKUP

后处理

  1. customThe ACN was evaporated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThis solution was washed with 1.0 N HCl, water, and brine
  4. dry with materialdried over sodium sulfate
  5. customthe solvent removed in vacuo
  6. washFlash column chromatography (eluting with a gradient from 0-80% ethyl acetate in hexanes)