HRID1594905

反应详情

EQUATION

反应方程式

HRID 1594905 的结构方程式

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

A solution of 1-allyl-3-ethyl-3-(3-methoxy-phenyl)-azepan-2-one (as described in Example 49, Step A) (0.9 g, 3.1 mmol) in MeOH (20 mL) at −78° C. was saturated with 03 for 20 min. The solution was warmed to −40° C. for 10 min then NaBH4 (0.36 g, 9.4 mmol) was added and the reaction mixture was stirred at 25° C. for 1 hr. The MeOH was removed in vacuo, and the residue was partitioned between EtOAc and saturated NaHCO3 solution. The organic layer was washed with brine and dried (MgSO4). Filtration and concentration to dryness gave the title compound.

WORKUP

后处理

  1. customThe MeOH was removed in vacuo
  2. customthe residue was partitioned between EtOAc and saturated NaHCO3 solution
  3. washThe organic layer was washed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationFiltration and concentration to dryness