HRID535313

反应详情

EQUATION

反应方程式

HRID 535313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-methoxy-N-methyl-2-oxopiperidine-4-carboxamide (2.72 g, 9.79 mmol) in THF (30 ml) was immersed in an ice-bath. MeMgBr (3M) in Et2O (4.57 ml, 13.70 mmol) was added slowly and the remaining white suspension was stirred for 1 h in an ice-bath and over night at room temperature. The reaction mixture was quenched carefully with aqueous saturated NaHCO3 and extracted with DCM. The organic layers were washed with brine, combined, dried over Na2SO4, filtered and concentrated in vacuo to obtain the title compound as yellow-brown oil. The crude product was directly used in the next step.

WORKUP

后处理

  1. customThe reaction mixture was quenched carefully with aqueous saturated NaHCO3
  2. extractionextracted with DCM
  3. washThe organic layers were washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo