HRID403506

反应详情

EQUATION

反应方程式

HRID 403506 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

In a argon flushed dry 25 ml 2-neckoundbottomflask (S)-2-methyl-4-oxo-piperidine-1-carboxylic acid tert-butyl ester (34) (0.6 g, 2.81 mmol) was dissolved in 10 ml of ether. A 1M solution of allylmagnesiumbromide in Et2O (3.66 ml, 3.66 mmol) was added dropwise at 0° C. The reaction mixture was stirred at 0° C. for 2 h. The mixture was quenched with NH4Cl solution and extracted with ether. The organic layer was washed with brine, dried over Na2 SO4 and evaporated. The crude product was purified by flash chromatography (silica gel, 20-30% EtOAc/cyclohexane) which furnished the product as white solid

WORKUP

后处理

  1. customIn a argon flushed
  2. customThe mixture was quenched with NH4Cl solution
  3. extractionextracted with ether
  4. washThe organic layer was washed with brine
  5. customdried over Na2 SO4
  6. customevaporated
  7. customThe crude product was purified by flash chromatography (silica gel, 20-30% EtOAc/cyclohexane) which