HRID586138

反应详情

EQUATION

反应方程式

HRID 586138 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The above alcohol (7.5 g, 40.0 mmol, 1.0 equiv) was dissolved in 500 mL of CH2Cl2. Pyridinium chlorochromate (12.96 g, 60.1 mmol, 1.5 equiv) was added and resulting mixture was stirred for 16 h. The dark liquid was decanted and the solvent was removed in vacuo. The residue was triturated with 500 mL of diethyl ether and the mixture was filtered. The filtrate was washed with 150 mL of 1 N HCl and dried over Na2SO4. The liquid was decanted and concentrated by rotary evaporation to yield 4-formyl-piperidine-1-carboxylic acid ethyl ester as a light brown oil (6.1 g).

WORKUP

后处理

  1. customresulting mixture
  2. customThe dark liquid was decanted
  3. customthe solvent was removed in vacuo
  4. customThe residue was triturated with 500 mL of diethyl ether
  5. filtrationthe mixture was filtered
  6. washThe filtrate was washed with 150 mL of 1 N HCl
  7. dry with materialdried over Na2SO4
  8. customThe liquid was decanted
  9. concentrationconcentrated by rotary evaporation