反应详情

To a 100 ml round bottomed flask was added 0.40 g (0.01 mole) of 60% sodium hydride. The sodium hydride was washed twice with hexane and 10 ml of dimethylformamide was added. Then, 2.1 g (0.05 mole) N,3-bis-(4-chlorophenyl)-4-methyl-4-phenyl-4,5-dihydro-1H-pyrazole-1-carboxamide (Example 2) was added portionwise. After hydrogen evolution ceased 1 ml of iodomethane was added and the mixture was stirred for 1 hour. The reaction mixture was partitioned between ether and water and the organic layer dried, filtered, concentrated, and chromatographed yielding 1.5 g of N,3-bis-(4-chlorophenyl)-N,4-dimethyl-4-phenyl-4,5-dihydro-1H-pyrazole-1-carboxamide. Mp 132°-135° C. NMR and IR data were consistent with the structure.

1. washThe sodium hydride was washed twice with hexane and 10 ml of dimethylformamide
2. additionwas added
3. additionwas added
4. customThe reaction mixture was partitioned between ether and water
5. customthe organic layer dried
6. filtrationfiltered
7. concentrationconcentrated
8. customchromatographed