반응 #2160380

반응 방정식

cyanogen bromide

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

dry-ice

sodium hydride

→

product

5-Amino-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one

용매

water

tetrahydrofuran

acetone

반응 조건

후처리

1. 1
   온도The reaction mixture temperature was maintained at -78° C. for 4 hours
2. 2
   온도to warm to room temperature over 16 hours
3. 3
   기타the solid which separated
4. 4
   기타was collected
5. 5
   세척washed with water and ether

실험 절차

To a stirred solution of 556 mg of 4,5-dihydro-7-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carboxamide (prepared as described in Example 4) in 25 ml of dry tetrahydrofuran, under nitrogen, cooled to -78° C. (dry-ice, acetone), was added 159 mg of sodium hydride (60% dispersion in mineral oil) in one portion. After stirring the mixture at -78° C. for 30 minutes, 191 mg of cyanogen bromide was added in one portion. The reaction mixture temperature was maintained at -78° C. for 4 hours, then was allowed to warm to room temperature over 16 hours. The mixture was diluted with water and the solid which separated was collected and washed with water and ether to give the product as a brown solid, m.p. 287°-289° C. (dec).

출처