HRID1269593
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
To a solution of ethyl 2-(4-formyl-2-methylphenoxy)-2-methylpropanoate (0.563 g, 2.25 mmol) in CH2Cl2 (10 mL) under nitrogen at room temperature, was added 4-trifluoromethylbenzyl amine (0.34 mL, 2.37 mmol). The resulting solution was stirred for 30 minutes prior to addition of sodium triacetoxyborohydride (0.668 g, 3.15 mmol). After 18 h stirring the reaction mixture was quenched by cautious addition of sat. sodium bicarbonate aq. (30 mL) and extracted CH2Cl2 (2×50 mL). The organic solution was dried (MgSO4) and the solvent removed in vacuo. Purification by SPE (Silica, 20 g) eluting 9:1 cyclohexane:EtOAc afforded the title compound as a colourless oil (0.485 g).
WORKUP
后处理
- stirringAfter 18 h stirring the reaction mixture
- customwas quenched by cautious addition of sat. sodium bicarbonate aq. (30 mL)
- extractionextracted CH2Cl2 (2×50 mL)
- dry with materialThe organic solution was dried (MgSO4)
- customthe solvent removed in vacuo
- customPurification by SPE (Silica, 20 g)
- washeluting 9:1 cyclohexane