HRID2294946
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturecooled
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in 50 mL of ice water
- washwashed with 50 mL of ether
- extractionextracted with 3×50 mL of chloroform
- dry with materialThe combined organic extracts were dried (MgSO4)
- concentrationconcentrated under reduced pressure
- customDrying under vacuum