HRID1426633

反应详情

EQUATION

反应方程式

HRID 1426633 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 (2.9 g, 9.2 mmol) and methyl (2E)-3-cyclopentylacrylate (1.70 g, 11.0 mmol) in ACN (100 mL), was added DBU (2.7 mL, 18 mmol). The resulting mixture was stirred for 96 hours. The ACN was removed in vacuo, and the resulting residue was dissolved in ethyl acetate. This solution was washed with 1.0 N HCl, followed by brine, and then dried over sodium sulfate, and the solvent removed in vacuo. Flash column chromatography (eluting with a gradient from 0-70% ethyl acetate in hexanes) afforded the product (2.73 g, 63%).

WORKUP

后处理

  1. customThe ACN was removed in vacuo
  2. dissolutionthe resulting residue was dissolved in ethyl acetate
  3. washThis solution was washed with 1.0 N HCl
  4. dry with materialdried over sodium sulfate
  5. customthe solvent removed in vacuo
  6. washFlash column chromatography (eluting with a gradient from 0-70% ethyl acetate in hexanes)