HRID47433

反应详情

EQUATION

反应方程式

HRID 47433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 7-bromoisatin (6.0 g) in acetone (27 ml) was treated with sodium hydroxide (4.6 g) in water (23 ml). The mixture was heated to reflux for 8 h, cooled and solvent reduced in volume at reduced pressure to approx. 25 ml. The residual aqueous phase was acidified with conc. HCl, extracted with ethyl acetate, the organic phase dried (MgSO4) and solvent removed at reduced pressure to give the title compound (7.2 g) as a yellow solid. 1H NMR δ: 2.85 (3H, s), 7.40 (1H, m), 7.90 (1H, s), 8.05 (1H, dd, J=1.2, 7.6 Hz), 8.79 (1H, dd, J=1.0, 8.5 Hz).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 8 h
  3. temperaturecooled
  4. extractionextracted with ethyl acetate
  5. dry with materialthe organic phase dried (MgSO4) and solvent
  6. customremoved at reduced pressure