HRID1052981
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
To concentrated H2SO4 (30 ml) at 65° C. was added N-(4-bromo-2-methoxyphenyl)-2-(hydroxyimino)acetamide (5.55 g, 20 mmol) portionwise. The mixture was heated at 90° C. for 1.5 h. The mixture was cooled to room temperature, poured onto ice, and stirred for 10 min. The solid was collected by filtration, washed with water, and air dried to afford 5-Bromo-7-methoxyindoline-2,3-dione (3.6 g, crude, 70% yield). This material was used without further purification. 1H NMR (400 MHz, DMSO-d6): δH 7.93 (s, 1H), 7.38 (s, 1H), 3.94 (s, 3H). MS (ESI) m/e [M+1]+ 256, 258.
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- additionpoured onto ice
- filtrationThe solid was collected by filtration
- washwashed with water, and air
- customdried