반응 #2454553

반응 방정식

4-bromo-2,6-difluorobenzonitrile

hydrazine

Hunig's base

→

title compound

6-Bromo-4-fluoro-1H-indazol-3-amine

용매

ethanol

반응 조건

후처리

1. 1
   기타Five batches of the below reaction
2. 2
   기타were run in sequence in a microwave reactor
3. 3
   기타The vial was capped
4. 4
   기타a yellow precipitate formed
5. 5
   기타The yellow precipitates
6. 6
   기타were collected
7. 7
   세척the solids were washed with cold ethanol

실험 절차

Five batches of the below reaction were run in sequence in a microwave reactor: To a 5-mL microwave vial was added 4-bromo-2,6-difluorobenzonitrile (3 g, 13.76 mmol), hydrazine (0.864 mL, 27.5 mmol), Hunig's base (4.81 mL, 27.5 mmol) and ethanol (10 mL). The vial was capped and stirred for 10 minutes at 150° C. in a microwave reactor. The reaction mixture was cooled (ice-water bath) and a yellow precipitate formed. The yellow precipitates were collected, combined and the solids were washed with cold ethanol to yield pale yellow rods of the title compound (13.0 g). LC-MS (ES) m/z=230 and 232 (1:1 intensity) [M+H]+.

출처