반응 #47277

반응 방정식

3-aminopyrazole

phthalic anhydride

water

→

2-(1H-pyrazol-3-yl)-isoindole-1,3-dione

수율 73.0%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONAfter addition
2. 2
   온도Upon cooling to 25° C.
3. 3
   기타which resulted in precipitation
4. 4
   온도The white suspension was cooled (−5° C.)
5. 5
   workup.STIRRINGstirred for 30 min
6. 6
   여과Subsequent filtration
7. 7
   세척washing with water, and suction
8. 8
   기타drying

실험 절차

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.

출처