HRID2269828

反应详情

EQUATION

反应方程式

HRID 2269828 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Combine of N,N′-di-(2-methylphenethyl)-2-((S)-2-(p-methoxybenzylmercapto)-3-phenylpropionylamino)malonamide (0.175 g, 0.274 mmol), mercury (II) acetate (0.108 g, 0.34 mmol), and anisole (0.3 mL) in dichloromethane (10 mL). Cool in an ice bath and degas by repeatedly applying vacuum and filling the vessel with nitrogen. Add trifluoroacetic acid (4 mL). After 3 hours, purge with hydrogen sulfide (gas) for about 10 minutes. Filter and evaporate in vacuo to give a residue. Combine the residue with carbon tetrachloride and evaporate in vacuo to remove most of the trifluoroacetic acid. Chromatograph the residue on silica gel eluting with 1/2 ethyl acetate/hexane and then 1/1 ethyl acetate/hexane to give the title compound.

WORKUP

后处理

  1. temperatureCool in an ice bath
  2. customdegas
  3. custompurge with hydrogen sulfide (gas) for about 10 minutes
  4. filtrationFilter
  5. customevaporate in vacuo
  6. customto give a residue
  7. customevaporate in vacuo
  8. customto remove most of the trifluoroacetic acid