HRID1264552

反应详情

EQUATION

反应方程式

HRID 1264552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Combine 2-(4-(2-(p-methoxybenzylthio)-6-phthalimidohexanoyl-amino)-3-oxo-1,3,4,5-tetrahydro-benzo[c]azepin-2-yl)-4-methyl-valeric acid t-butyl ester (0.20 mmol), mercury (II) acetate (0.084 g, 0.26 mmol), and anisole (0.23 mL, 2.1 mmol) in dichloromethane (6.6 mL). Cool in an ice bath and degas by repeatedly cycles of vacuum and filling the vessel with nitrogen gas. Add trifluoroacetic acid (2.5 mL). After 1 hour, warm to ambient temperature. After 3 hours, purge with hydrogen sulfide (gas) for about 10 minutes. Filter and evaporate in vacuo to give a residue. Repeatedly, combine the residue and carbon tetrachloride and evaporate in vacuo to give the title compound.

WORKUP

后处理

  1. temperatureCool in an ice bath
  2. customdegas by repeatedly cycles of vacuum
  3. waitAfter 3 hours
  4. custompurge with hydrogen sulfide (gas) for about 10 minutes
  5. filtrationFilter
  6. customevaporate in vacuo
  7. customto give a residue
  8. customevaporate in vacuo