HRID1269590

反应详情

EQUATION

反应方程式

HRID 1269590 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 (4-formyl-2-methylphenoxy)acetate (3 g, 13.5 mmol) in anhydrous ethanol (50 mL) at room temperature, was added n-butylamine (1.6 mL, 16.2 mmol) and 4A molecular sieves. The resultant mixture was stirred at room temperature for 18 h under nitrogen, prior to portion wise addition of sodium triacetoxyborohydride (3.43 g, 16.2 mmol). After a further 3 h stirring at room temperature, the reaction was quenched by cautious addition of sat. sodium bicarbonate solution (40 mL) and then diluted with water (50 mL), before extracting with EtOAc (2×100 mL). The combined organic extracts were dried (MgSO4) and the solvents removed in vacuo, to afford the title compound as brown oil (2.6 g).

WORKUP

后处理

  1. customthe reaction was quenched by cautious addition of sat. sodium bicarbonate solution (40 mL)
  2. additiondiluted with water (50 mL)
  3. extractionbefore extracting with EtOAc (2×100 mL)
  4. dry with materialThe combined organic extracts were dried (MgSO4)
  5. customthe solvents removed in vacuo