HRID262346

反应详情

EQUATION

反应方程式

HRID 262346 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 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

  1. additionwas added, in portions, 10 g
  2. additionAfter the addition
  3. extractionextracted with EtOAc
  4. dry with materialThe organic phase was dried (MgSO4)
  5. concentrationconcentrated
  6. customthe residue chromatographed on silica gel