HRID1165276

反应详情

EQUATION

反应方程式

HRID 1165276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-bromo-1-[3-(methoxymethyl)-4-(phenylmethoxy)phenyl]ethanone (2.0 g), dibenzylamine (1.2 g) and DEA (0.8 g) in THF (30 ml) was allowed to stand at room temperature for 18 h, filtered and evaporated. The residual oil was dissolved in ethanol (20 ml) and treated portionwise with sodium borohydride (0.23 g), under nitrogen. The mixture was stirred at room temperature for 1 h, treated with methanol (20 ml), and evaporated. The residue was purified by FCC eluting with CX-ER (3:1) to give the title compound as an off-white solid (2.3 g), m.p. 52°-57°, t.l.c. (CX-ER 1:1) Rf 0.5

WORKUP

后处理

  1. filtrationfiltered
  2. customevaporated
  3. dissolutionThe residual oil was dissolved in ethanol (20 ml)
  4. additiontreated portionwise with sodium borohydride (0.23 g), under nitrogen
  5. additiontreated with methanol (20 ml)
  6. customevaporated
  7. customThe residue was purified by FCC
  8. washeluting with CX-ER (3:1)