HRID427714

反应详情

EQUATION

反应方程式

HRID 427714 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirring solution of 1-Boc-4-methoxycarbonyl-3,4-didehydropiperidine (28.81 g, 119 mmol) in methanol (300 mL) was added 1 N aqueous sodium hydroxide (300 mL). After stirring overnight, the solvent was removed by rotary evaporation and the residue was partitioned between water and diethyl ether. The aqueous phase was separated and washed with diethyl ether, acidified to pH 2.5 with conc. HCl, then extracted with diethyl ether. The organic extract was then washed with brine, dried with MgSO4, filtered and concentrated in vacuo to give 25.16 g (93%) of a light yellow solid.

WORKUP

后处理

  1. customthe solvent was removed by rotary evaporation
  2. customthe residue was partitioned between water and diethyl ether
  3. customThe aqueous phase was separated
  4. washwashed with diethyl ether
  5. extractionextracted with diethyl ether
  6. extractionThe organic extract
  7. washwas then washed with brine
  8. dry with materialdried with MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo