HRID236729
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
PROCEDURE
实验过程
To a solution of 90 ml. of CF3CO2H and 15 ml. of H2O, cooled to -20° was added, in portions, 10 g. (0.022 mol) of the end product of Example 20. After the addition was complete, the solution was stirred at -15° to -20° for 1 hour, poured into excess saturated K2CO3 solution and extracted with EtOAc. The organic phase was dried (MgSO4), concentrated and the residue chromatographed on silica gel to give the end product as a pale yellow oil. The analytical sample was obtained as a colorless oil by bulb to bulb distillation: bp 175 (0.05 mm).
WORKUP
后处理
- additionwas added, in portions, 10 g
- additionAfter the addition
- extractionextracted with EtOAc
- dry with materialThe organic phase was dried (MgSO4)
- concentrationconcentrated
- customthe residue chromatographed on silica gel