反应 #44892

反应方程式

oxalic acid

2-(1H-Indol-3-ylsulfanyl)-N,N-dimethyl benzamide

borane

Methanol

→

[2-(1H-Indol-3-ylsulfanyl)benzyl]dimethyl amine

溶剂

tetrahydrofuran

tetrahydrofuran

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture stirred at room temperature for 30 min
2. 2
   其他evaporated in vacuo
3. 3
   workup.DISSOLUTIONThe mixture was redissolved in ethyl acetate (100 mL)
4. 4
   洗涤washed with saturated sodium hydrogen carbonate (20 mL)
5. 5
   干燥dried over anhydrous MgSO4
6. 6
   其他evaporated in vacuo
7. 7
   其他The product was crystallized as an oxalate salt by dissolution in acetone

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.

来源