HRID1269593

反应详情

EQUATION

反应方程式

HRID 1269593 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringAfter 18 h stirring the reaction mixture
  2. customwas quenched by cautious addition of sat. sodium bicarbonate aq. (30 mL)
  3. extractionextracted CH2Cl2 (2×50 mL)
  4. dry with materialThe organic solution was dried (MgSO4)
  5. customthe solvent removed in vacuo
  6. customPurification by SPE (Silica, 20 g)
  7. washeluting 9:1 cyclohexane