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-(Bromoacetyl)furan (95 g) is added slowly to a stirred mixture of 75 g of N-methylbenzylamine and 70 g of potassium carbonate in 300 ml of methanol at 20°-30° C. The mixture is stirred at room temperature for 2.5 hours, and the insoluble matter is filtered off. To the filtrate is added 20 g of sodium borohydride at 10°-20° C. with stirring, and the mixture is stirred at room temperature for 3 hours. The solvent is then distilled off under reduced pressure, water is added to the residue, and the separated oil is extracted with ethyl acetate. The extract is washed with water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. Distillation of the residue gives 80 g of 2-(N-benzyl-N-methylamino)-1-(2-furyl)ethanol as pale yellow viscous oil, boiling at 130°-138° C. (0.2 mmHg).
WORKUP
后处理
- filtrationthe insoluble matter is filtered off
- additionTo the filtrate is added 20 g of sodium borohydride at 10°-20° C.
- stirringwith stirring
- stirringthe mixture is stirred at room temperature for 3 hours
- distillationThe solvent is then distilled off under reduced pressure, water
- additionis added to the residue
- extractionthe separated oil is extracted with ethyl acetate
- washThe extract is washed with water
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- distillationDistillation of the residue