HRID2269814

反应详情

EQUATION

反应方程式

HRID 2269814 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Combine N,N′-diphenethyl-2-((R)-2-bromo-3-methylbutyrylamino)malonamide (0.20 g, 0.41 mmol), thioacetic acid (0.08 mL, 1.1 mmol), and dimethylformamide (8 mL). Degas by repeated cycles of vacuum and filling with nitrogen gas. Add cesium carbonate (0.215 g, 0.664 mmol). After 18 hours, dilute with water and extract with ethyl acetate. Extract the organic layer with brine, dry over Na2SO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with 1/1 hexane ethyl acetate to give the title compound.

WORKUP

后处理

  1. customDegas by repeated cycles of vacuum
  2. extractionextract with ethyl acetate
  3. extractionExtract the organic layer with brine
  4. dry with materialdry over Na2SO4
  5. filtrationfilter
  6. customevaporate in vacuo
  7. customto give a residue