HRID16614
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringthe mixture stirred at room temperature for 30 min
- customevaporated in vacuo
- dissolutionThe mixture was redissolved in ethyl acetate (100 mL)
- washwashed with saturated sodium hydrogen carbonate (20 mL)
- dry with materialdried over anhydrous MgSO4
- customevaporated in vacuo
- customThe product was crystallized as an oxalate salt by dissolution in acetone