HRID1717669

反应详情

EQUATION

反应方程式

HRID 1717669 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 6-Bromo-2-(2,4-dichloro-benzoyl)-benzofuran-3-one (3.30 g, 8.55 mmol) in acetone (50 mL) was added dimethyl sulfate (1.19 g, 9.40 mmol) and cesium carbonate (4.18 g, 12.82 mmol). The resulting mixture was heated at 50 deg for 6 hours is at which time the reaction mixture was concentrated via rotary evaporation. The resulting mixture was taken up in EtOAc and washed twice with water and one time with a saturated sodium carbonate solution. The organic portion was dried over MgSO4 and then filtered and concentrated. The resultant oil was purified via column chromatography (10% MeOH/Dichloromethane) to provide the title compound (950 mg, 28%). 1H-NMR (CDCl3): δ 8.03 (d, 1H), 7.65 (d, 1H), 7.46 (m, 2H), 7.35 (m, 2H), 2.46 (s, 3H).

WORKUP

后处理

  1. temperatureThe resulting mixture was heated at 50 deg for 6 hours
  2. concentrationwas concentrated via rotary evaporation
  3. washwashed twice with water and one time with a saturated sodium carbonate solution
  4. dry with materialThe organic portion was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe resultant oil was purified via column chromatography (10% MeOH/Dichloromethane)