HRID349658

反应详情

EQUATION

反应方程式

HRID 349658 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of sodium borohydride (NaBH4) (0.66 g, 17 mmol) in water (25 mL) was treated with 4-morpholinylsalicylaldehyde (1.8 g, 9 mmol) in small portions over 30 min and stirred at room temperature for 3 h. The reaction was quenched with acetone (5.1 mL, 100 mmol), acidified to pH 7 with 7.8 mL of 5% hydrochloric acid (aqueous) and extracted with chloroform (CHCl3) (2×100 mL). The combined CHCl3 extracts were dried over sodium sulfate (Na2SO4) and concentrated in vacuo to yield 0.7 g of pale yellow solid which was purified by trituration with 60/40 CHCl3/ethyl acetate (EtOAc) to yield the product as a white solid (0.25 g).

WORKUP

后处理

  1. extractionextracted with chloroform (CHCl3) (2×100 mL)
  2. dry with materialThe combined CHCl3 extracts were dried over sodium sulfate (Na2SO4)
  3. concentrationconcentrated in vacuo