HRID2294946

反应详情

EQUATION

反应方程式

HRID 2294946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 200 mg of ethyl 2-tert-butoxycarbonylamino-5-pyrimidinecarboxylate, 125 mg of potassium hydroxide and 15 mL of ethanol was heated to 70° C. for 3 h, cooled and concentrated under reduced pressure. The residue was dissolved in 50 mL of ice water, washed with 50 mL of ether, acidified to pH=3 with conc. HCl and extracted with 3×50 mL of chloroform. The combined organic extracts were dried (MgSO4) and concentrated under reduced pressure. Drying under vacuum gave 156 mg of 2-tert-butoxycarbonylamino-5-pyrimidinecarboxylic acid as a white solid.

WORKUP

后处理

  1. temperaturecooled
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue was dissolved in 50 mL of ice water
  4. washwashed with 50 mL of ether
  5. extractionextracted with 3×50 mL of chloroform
  6. dry with materialThe combined organic extracts were dried (MgSO4)
  7. concentrationconcentrated under reduced pressure
  8. customDrying under vacuum