HRID1993377

反应详情

EQUATION

反应方程式

HRID 1993377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(3-fluoro-4-methoxyphenyl)-4-(phenoxymethyl)pyrrolidin-2-one (Step 3, 1.0 g, 3.17 mmol) in 15.85 mL of 1 M BBr3/CH2Cl2 was stirred at RT for 10 h. The solution was concentrated in vacuo and the residue was diluted with 100 mL of EtOAc. The organic phase was washed with 40 mL of satd. NaHCO3 followed by 40 mL of brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by chromatography (5% to 60% EtOAc/hexane) to give the title compound as a light yellow foam. MS (ESI pos. ion) m/z: 302.3 (M+H). Calc'd Exact Mass for C17H16FNO3: 301.31.

WORKUP

后处理

  1. concentrationThe solution was concentrated in vacuo
  2. additionthe residue was diluted with 100 mL of EtOAc
  3. washThe organic phase was washed with 40 mL of satd
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by chromatography (5% to 60% EtOAc/hexane)