HRID1771429

反应详情

EQUATION

反应方程式

HRID 1771429 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 1-(2-bromophenyl)-4,4,4-trifluorobutan-2-one (7.0 g, 24.9 mmol) in MeOH (150 ml) was added NaBH4 (1.23 g, 32.3 mmol) at 0° C. and stirred for 1 h at RT. Then the reaction mixture was quenched with MeOH and concentrated under reduced pressure to afford crude compound. The title compound was purified by separation methods A, E and H. (Yield 1.6 g of Enantiomer-1 and 1.4 g-Enantiomer-2). The enantiomer-1 showed up at tr=5.67 min and enantiomer-2 showed up at tr=9.57 min with Chiralcel OD-H (4.6×250 mm) 5μ, hexane:2-PrOH:TFA (90:10:0.1), 1 ml/min.

WORKUP

后处理

  1. customThen the reaction mixture was quenched with MeOH
  2. concentrationconcentrated under reduced pressure
  3. customto afford crude compound
  4. customThe title compound was purified by separation methods A, E and H
  5. customshowed up at tr=5.67 min and enantiomer-2
  6. customshowed up at tr=9.57 min with Chiralcel OD-H (4.6×250 mm) 5μ, hexane:2-PrOH:TFA (90:10:0.1), 1 ml/min.