HRID1395821

反应详情

EQUATION

反应方程式

HRID 1395821 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.0 g of t-butoxycarbonylsarcosylnitroarginylvalyltyrosylisoleucylhistidylprolylserine methyl ester is dissolved in 20 ml of pyridine and 10 ml of triethylamine. The solution is cooled in an ice bath. 0.51 g of tosyl chloride is added to the solution. At ten minute intervals, three additional 0.51 g batches of tosyl chloride are added. After standing for two hours, the reaction mixture is filtered. 200 ml of methylene chloride is added to the reaction. The solution is extracted three times with 5% ammonium hydroxide in water. The solution is then dried over sodium sulfate and stripped under vacuum. The residue istaken up in 2% methanol/methylene chloride and passed through a silica gel column to remove the colored impurities and afford the pure product t-butoxycarbonylsarcosylnitroarginylvalyltyrosylisoleucylhistidylprolyldehydroalanine methyl ester.

WORKUP

后处理

  1. temperatureThe solution is cooled in an ice bath
  2. filtrationthe reaction mixture is filtered
  3. addition200 ml of methylene chloride is added to the reaction
  4. extractionThe solution is extracted three times with 5% ammonium hydroxide in water
  5. dry with materialThe solution is then dried over sodium sulfate
  6. customto remove the colored impurities