HRID1351550

反应详情

EQUATION

反应方程式

HRID 1351550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 5 g of 4-(N-methoxy-N-methyl-carbamoyl)-piperidine-1-carboxylic acid benzyl ester (S. Nahm and S. W. Weinreb, Tetrahedron Letters, 22:3815–3818(1981)) in 50 mL of anhydrous THF cooled to 0° C., was added dropwise 6 mL of 3M methylmagnesium bromide in ether over 10 minutes. After stirring for 1 h at 0° C., the resulting mixture was quenched with 50 mL of 1N HCl and extracted with 3×50 mL of ether. The combined extracts were dried over magnesium sulfate and concentrated to dryness under reduced pressure. Drying under vacuum gave 4-Acetyl-piperidine-1-carboxylic acid benzyl ester as a white solid:

WORKUP

后处理

  1. customthe resulting mixture was quenched with 50 mL of 1N HCl
  2. extractionextracted with 3×50 mL of ether
  3. dry with materialThe combined extracts were dried over magnesium sulfate
  4. concentrationconcentrated to dryness under reduced pressure
  5. customDrying under vacuum