HRID455544

反应详情

EQUATION

反应方程式

HRID 455544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(Boc-amino)-N-{1-[1-(4-chlorophenyl)cyclobutyl]-3-methylbutyl}-3-methylvaleramide (Example 2) was dissolved in CF3COOH. This solution was stirred at room temperature for 3 hours, and then evaporated under vacuum to remove CF3COOH. The produced white solid was collected, dissolved in anhydrous ethyl ether, and washed repeatedly with saturated sodium bicarbonate until pH of the eluate was neutral. This solution of ethyl ether was then washed with saturated sodium chloride for 2-3 times, dried over anhydrous sodium sulfate, and concentrated. The crude product was purified by column chromatography to give 2-amino-N-{1-[1-(4-chlorophenyl)cyclobutyl]-3-methylbutyl}-3-methylvaleramide.

WORKUP

后处理

  1. customevaporated under vacuum
  2. customto remove CF3COOH
  3. customThe produced white solid was collected
  4. dissolutiondissolved in anhydrous ethyl ether
  5. washwashed repeatedly with saturated sodium bicarbonate until pH of the eluate
  6. washThis solution of ethyl ether was then washed with saturated sodium chloride for 2-3 times
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated
  9. customThe crude product was purified by column chromatography