HRID1765364

反应详情

EQUATION

反应方程式

HRID 1765364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

4-Isopropyl phenyl hydrazine hydrochloride (2.77 g, 14.6 mmol) was added in one portion to a stirred mixture of phthalic anhydride (2.0 g, 13 mmol) in acetic acid (25 ml) at room temperature. The reaction mixture was heated to 125° C. for 2 hours, and then allowed to cool to room temperature. The resultant suspension was poured into H2O (100 ml), NaHCO3 solution (1M) was added and the resulting solid was removed by filtration. The mother liquor was acidified with conc. HCl The resulting solid was collected by filtration and dried in vacuum to give the title compound (1.62 g, 45% yield) as a white solid. 1H-NMR: (400 MHz, D6-DMSO) 11.80 (1H, s), 8.30 (1H, d), 7.92–8.01 (3H, m), 7.92 (2H, d), 7.35 (2H, d), 2.96 (1H, m), 1.25 (6H, d); MS (ESI+)=345.12 (M+H)+.

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. additionwas added
  3. customthe resulting solid was removed by filtration
  4. filtrationwas collected by filtration
  5. customdried in vacuum