반응 #2137691

반응 방정식

4,5-dihydro-7-(3-(trifluoromethyl)phenyl)pyrazolo(1,5-a)pyrimidine-3-carboxamide

4,5-Dihydro-7-(3-(trifluoromethyl)phenyl)-pyrazolo(1,5 -a)pyrimidine-3-carboxamide

1,1'-carbonyldiimidazole

→

desired product

수율 59.9%

8-(3-(Trifluoromethyl)phenyl)-3H,6H-1,4,5a,8a-tetraazaacenaphthylene-3,5(4H)-dione

수율 59.9%

용매

dioxane

반응 조건

후처리

1. 1
   온도The mixture is then heated
2. 2
   온도at reflux for 5 hours
3. 3
   온도is cooled
4. 4
   여과filtered
5. 5
   기타The filtrate is evaporated to dryness in vacuo
6. 6
   workup.ADDITIONan excess of water is added to the residue
7. 7
   기타The white solid which forms is collected
8. 8
   기타is recrystallized from acetonitrile-ethanol

실험 절차

To a stirred mixture of 10.0 g of 4,5-dihydro-7-(3-(trifluoromethyl)phenyl)pyrazolo(1,5-a)pyrimidine-3-carboxamide (prepared as described in Example 8) in 200 ml of dioxane at room temperature under nitrogen is added 20.0 g of 1,1'-carbonyldiimidazole. The mixture is then heated at reflux for 5 hours, and then is cooled and filtered. The filtrate is evaporated to dryness in vacuo and an excess of water is added to the residue. The white solid which forms is collected and is recrystallized from acetonitrile-ethanol to give 6.5 g of the desired product as a white solid, mp 260-262° C.

출처