반응 #2137697

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

sodium hydride

1,1'-thiocarbonyldiimidazole

→

desired product

수율 82.2%

4,5-Dihydro-5-thioxo-8-(3-(trifluoromethyl)phenyl)-3H,6H-1,4,5a,8a-tetraazaacenaphthylene-3-one

수율 82.2%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도to slowly warm to room temperature
2. 2
   workup.STIRRINGis stirred for 36 hours
3. 3
   기타The mixture is quenched with water
4. 4
   추출extracted with chloroform
5. 5
   기타Evaporation of the
6. 6
   추출extract in vacuo

실험 절차

To a stirred solution of 1.00 g of 4,5-dihydro-7-(3-(trifluoromethyl)phenyl)pyrazolo(1,5-a)pyrimidine-3-carboxamide (prepared as described in Example 8) in 30 ml of dry tetrahydrofuran cooled to -78° C. is added 286 mg of 60 percent sodium hydride (dispersion in mineral oil). The reaction mixture is stirred at -78° C. for 30 minutes then 637 mg of 1,1'-thiocarbonyldiimidazole is added and the mixture is allowed to slowly warm to room temperature and then is stirred for 36 hours. The mixture is quenched with water, neutralized with 5 percent aqueous hydrochloric acid and extracted with chloroform. Evaporation of the extract in vacuo gives 934 mg of the desired product.

출처