反応 #44892

反応方程式

oxalic acid

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

borane

Methanol

→

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

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

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

実験手順

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.

出典