HRID601092

反应详情

EQUATION

反应方程式

HRID 601092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 2,4-bis(tert-butyl)-6-[[(2,6-dibromophenyl)imino]methyl]phenol (0.91 g, 2.41 mmol) in methanol (20 ml) was added NaBH4 (1.2 g), in small portions. The yellow suspension was stirred for 2 hours during which the yellow solution turned clear. Water (10 ml) was then slowly added, the organic phase separated and the aqueous phase extracted with dichloromethane (3×10 ml). The organic fractions were combined, dried (NaSO4), and the solvent removed under reduced pressure. The crude product was purified by recrystallisation from hot hexane to afford the product as large colourless crystals. Yield 0.48 g, 95%.

WORKUP

后处理

  1. customthe organic phase separated
  2. extractionthe aqueous phase extracted with dichloromethane (3×10 ml)
  3. dry with materialdried (NaSO4)
  4. customthe solvent removed under reduced pressure
  5. customThe crude product was purified by recrystallisation from hot hexane