HRID1681150

反应详情

EQUATION

反应方程式

HRID 1681150 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A portion of the Orude -acetyl 9-benzyl-1,2,3,4-tetrahydro-β-carboline (1.7 g) was heated at reflux for 4.5 hours in 2 N NaOH (50 mL) in methanol:water 2:3, v/v). The methanol was removed by evaporation under vacuum, and the crude 9-benzyl-1,2,3,4-tetrahydro-β-carboline free base was extracted into chloroform. This extract was dried over anhydrous MgSO4, filtered, and the filtrate evaporated under vacuum. The hydrochloride salt was prepared by passing dry HCl through a solution of the crude free base in diethyl ether. The resulting precipitate was filtered and recrystallized from acetonitrile to yield pure 9-benzyl-1,2,3,4-tetrahydro-β-carboline.

WORKUP

后处理

  1. customThe methanol was removed by evaporation under vacuum
  2. extractionthe crude 9-benzyl-1,2,3,4-tetrahydro-β-carboline free base was extracted into chloroform
  3. dry with materialThis extract was dried over anhydrous MgSO4
  4. filtrationfiltered
  5. customthe filtrate evaporated under vacuum
  6. filtrationThe resulting precipitate was filtered
  7. customrecrystallized from acetonitrile