HRID18999

反应详情

EQUATION

反应方程式

HRID 18999 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

To a stirred mixture of 3-aminopyrazole (5.00 g, 60.2 mmol) dissolved in N,N-dimethylformamide (75 mL) was added phthalic anhydride (8.91 g, 60.2 mmol). After addition was complete, the mixture was stirred at 125° C. for 24 h. Upon cooling to 25° C., water (100 mL) was added, which resulted in precipitation. The white suspension was cooled (−5° C.) and stirred for 30 min. Subsequent filtration, washing with water, and suction drying afforded 2-(1H-pyrazol-3-yl)-isoindole-1,3-dione (9.36 g, 73.0%) as a white solid: LR-ES-MS m/z calculated for C11H7N3O2 [M]+ 213, observed [M+H]+ 214.

WORKUP

后处理

  1. additionAfter addition
  2. temperatureUpon cooling to 25° C.
  3. customwhich resulted in precipitation
  4. temperatureThe white suspension was cooled (−5° C.)
  5. stirringstirred for 30 min
  6. filtrationSubsequent filtration
  7. washwashing with water, and suction
  8. customdrying