反应详情

To a stirred solution of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole (5.0 g) in acetonitrile (60 ml) at room temperature was added N-iodosuccinimide (3.52 g), portionwise over a period of five minutes. Stirring was continued for 1 hr and the mixture was then evaporated to dryness to provide the crude product (8.2 g), still containing succinimide. This may be used without further purification or, if desired, purified by partitioning between dichloromethane and water, separating, drying (MgSO4) and evaporating the organic layer to produce a yellow solid. Trituration with hexane provides the title compound as a white solid, m.p. 213° C. (decomp.).

1. waitwas continued for 1 hr
2. customthe mixture was then evaporated to dryness
3. customto provide the crude product (8.2 g), still containing succinimide
4. customThis may be used without further purification
5. custompurified
6. customby partitioning between dichloromethane and water
7. customseparating
8. dry with materialdrying (MgSO4)
9. customevaporating the organic layer
10. customto produce a yellow solid