HRID926703

反应详情

EQUATION

反应方程式

HRID 926703 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl magnesium bromide (3.0M in Diethyl ether) (1.5 mL, 4.5 mmol) was added to cold (−10° C.) solution of tert-butyl 3-oxoazetidine-1-carboxylate (650 mg, 3.8 mmol) in THF (10 mL) and stirring was continued at 20-35° C. for 1 h. After which the reaction mixture was quenched with saturated aqueous NH4Cl solution and extracted with ethylacetate. The organic layer separated was washed with water, dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford the residue. The residue was purified by column chromatography (using 60-120 silica gel and 50% EtOAc in Hexane as eluent) to afford 430 mg of the title compound.

WORKUP

后处理

  1. customAfter which the reaction mixture was quenched with saturated aqueous NH4Cl solution
  2. extractionextracted with ethylacetate
  3. customThe organic layer separated
  4. washwas washed with water
  5. dry with materialdried over anhydrous sodium sulphate
  6. concentrationconcentrated under reduced pressure
  7. customto afford the residue
  8. customThe residue was purified by column chromatography (using 60-120 silica gel and 50% EtOAc in Hexane as eluent)