HRID926005

反应详情

EQUATION

反应方程式

HRID 926005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cold solution of compound 38 (1.80 mmol), TBTU (2.17 mmol), and N-methylhex-5-en-1-amine tosylate salt 31a (2.17 mmol) in DMF (100 mL) was added diisopropyl ethyl amine (5.4 mmol) dropwise under nitrogen at 0° C. The reaction mixture was stirred overnight at room temperature, then quenched with water and extracted with diethyl ether. The organic layer was washed with brine, then dried on magnesium sulphate, concentrated under reduced pressure, and purified by chromatography on silica gel to yield compound 39 as a beige solid in 85% yield. MS (ESI, EI+): m/z=578 (MH+).

WORKUP

后处理

  1. customquenched with water
  2. extractionextracted with diethyl ether
  3. washThe organic layer was washed with brine
  4. customdried on magnesium sulphate
  5. concentrationconcentrated under reduced pressure
  6. custompurified by chromatography on silica gel