HRID1396135

反应详情

EQUATION

反应方程式

HRID 1396135 的结构方程式

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

4-Chloro-7H-pyrrolo[2,3-d]pyrimidine (9, 300 mg, 1.95 mmol) is combined with 3.00 mL of ethanol (10, 51.4 mmol), then potassium hydroxide (0.226 g, 4.03 mmol) is added. The reaction is heated at 120° C. for 3 hours in a microwave, then extracted with ethyl acetate and aqueous saturated ammonium chloride. The organic layer is washed with brine, dried with magnesium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material is recrystallized from methanol to provide the desired compound (11, 213 mg). MS (ESI) [M+H+]+=164.9.

WORKUP

后处理

  1. extractionextracted with ethyl acetate and aqueous saturated ammonium chloride
  2. washThe organic layer is washed with brine
  3. dry with materialdried with magnesium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated under vacuum
  6. customThe resulting material is recrystallized from methanol