Dimethyl Sulfate → 3,4,5-Tribromo-1-methyl-1H-pyrazole

반응식

[Br:1][C:2]1[C:6]([Br:7])=[C:5]([Br:8])[NH:4][N:3]=1.[OH-].[Na+].S(OC)(O[CH3:15])(=O)=O>>[Br:1][C:2]1[C:6]([Br:7])=[C:5]([Br:8])[N:4]([CH3:15])[N:3]=1

참가 물질

반응물 3

HCID 6497Dimethyl Sulfate2회

HCID 14798Sodium Hydroxide

HCID 6276743,4,5-tribromo-1H-pyrazole

생성물 1

HCID 133340543,4,5-Tribromo-1-methyl-1H-pyrazole

실험 절차

To 3,4,5-tribromopyrazole (4.5 g, 0.15 mole) in 3N aqueous sodium hydroxide (6 g, 0.15 mole) is added at room temperature with stirring dimethyl sulfate (19 g, 0.15 mole). After 10 minutes a solid separates out. An additional gram of dimethyl sulfate is added and the mixture is stirred for 3 days, filtered and the precipitate water washed and air dried to yield 33 g (73%), mp 85° C. to 86° C. Crystallization from cyclohexane yields desired solid product whose melting point ranges from about 90° C. to 91° C.