HRID921969

反应详情

EQUATION

反应方程式

HRID 921969 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 6-bromo-8-fluoro-3,4-dihydroquinolin-2(1H)-one (1-3, 2.00 g, 8.19 mmol) in toluene (50 mL) was added Lawesson's reagent (1.66 g, 4.10 mmol). After refluxing the reaction mixture for 2 h, the toluene was distilled off to yield the crude product, which was then purified by flash chromatography on silica gel to obtain the title compound as a yellow solid; 1H NMR (DMSO-D6, 500 MHz) δ=12.14 (s, 1H), 7.46 (dd, J=2.0 Hz, JHF=10.0 Hz, 1H), 7.34 (s, 1H), 2.94 (d, J=8.0 Hz, 2H), 2.84 (d, J=8.0 Hz, 2H).

WORKUP

后处理

  1. temperatureAfter refluxing the reaction mixture for 2 h
  2. distillationthe toluene was distilled off
  3. customto yield the crude product, which
  4. customwas then purified by flash chromatography on silica gel