HRID1988189

反应详情

EQUATION

反应方程式

HRID 1988189 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-(Bromomethyl)-4-(4-fluorophenyl)-2H-chromen-2-one can be prepared as described in Example 1A; its preparation is also described in U.S. Pat. No. 5,552,437. 7-(Bromomethyl)-4-(4-fluorophenyl)-2H-chromen-2-one (11.42 g, 34.3 mmol) and NMO (13.9 g, 102.8 mmol) in 110 mL of dioxane were heated to reflux for 6 h. The solution was cooled to rt and the solvent removed. The crude compound was diluted in EtOAc and washed with NH4Claq, water, brine and dried over MgSO4. The solvent was removed to yield the title compound. 1H NMR (400 MHz, acetone-d6): δ 10.20 (1H, s), 7.95 (1H, s), 7.85 (1H, m), 7.68 (3H, m), 7.38 (2H, m) and 6.51 (1H, s).

WORKUP

后处理

  1. customits preparation
  2. temperatureto reflux for 6 h
  3. customthe solvent removed
  4. additionThe crude compound was diluted in EtOAc
  5. washwashed with NH4Claq, water, brine
  6. dry with materialdried over MgSO4
  7. customThe solvent was removed