HRID16614

反应详情

EQUATION

反应方程式

HRID 16614 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(1H-Indol-3-ylsulfanyl)-N,N-dimethyl benzamide (1 mmol) was dissolved in dry tetrahydrofuran (30 mL). To the mixture was added 3 mL 1 M borane in tetrahydrofuran and the mixture was stirred at room temperature for 24 hours. Methanol (5 mL) was added and the mixture stirred at room temperature for 30 min and then evaporated in vacuo. The mixture was redissolved in ethyl acetate (100 mL) and washed with saturated sodium hydrogen carbonate (20 mL), dried over anhydrous MgSO4 and evaporated in vacuo. The product was crystallized as an oxalate salt by dissolution in acetone and addition of one equivalent of oxalic acid.

WORKUP

后处理

  1. stirringthe mixture stirred at room temperature for 30 min
  2. customevaporated in vacuo
  3. dissolutionThe mixture was redissolved in ethyl acetate (100 mL)
  4. washwashed with saturated sodium hydrogen carbonate (20 mL)
  5. dry with materialdried over anhydrous MgSO4
  6. customevaporated in vacuo
  7. customThe product was crystallized as an oxalate salt by dissolution in acetone