Ammonia → Rufinamide
반응식
[F:1][C:2]1[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[C:3]=1[CH2:4][N:5]1[CH:9]=[C:8]([C:10](O)=[O:11])[N:7]=[N:6]1.S(Cl)(Cl)=O.[NH3:22]>>[CH:15]1[CH:14]=[C:13]([F:17])[C:3]([CH2:4][N:5]2[N:6]=[N:7][C:8]([C:10]([NH2:22])=[O:11])=[CH:9]2)=[C:2]([F:1])[CH:16]=1참가 물질
반응 조건
- 온도
- 80 °C
실험 절차
A mixture of 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-carboxylic acid (25 gms) and thionyl chloride (63.5 gms) were stirred at 80° C. and maintained for 3 hours. The reaction mass was cooled to 50° C. and excess thionyl chloride was distilled off. To this reaction mass toluene (25 ml) was charged twice and it was distilled off under vacuum it was followed by addition of toulene (175 ml) to get clear solution. Aqueous ammonia (100 ml) charged into reaction mass at room temperature and maintained for 2 hours. The reaction mass was filtered. 10% sodium carbonate solution was added to above solid and stirred for 30 minutes. The solid was filtered and washed with water and cyclohexane (50 ml). Dried the crude material in a vacuum oven at 70-80° C. for 10 hours. Yield: 23.00 gm.
후처리
- temperaturemaintained for 3 hours
- temperatureThe reaction mass was cooled to 50° C.
- distillationexcess thionyl chloride was distilled off
- additionTo this reaction mass toluene (25 ml) was charged twice
- distillationit was distilled off under vacuum it
- additionwas followed by addition of toulene (175 ml)
- customto get clear solution
- temperaturemaintained for 2 hours
- filtrationThe reaction mass was filtered
- addition10% sodium carbonate solution was added to above solid
- stirringstirred for 30 minutes
- filtrationThe solid was filtered
- washwashed with water and cyclohexane (50 ml)
- dry with materialDried the crude material in a vacuum oven at 70-80° C. for 10 hours
출처 및 근거
- ORD 기록
- ord-4265b18b507e4fb8aae24dcb0eb4fdad
- 출처 데이터셋
- uspto-grants-2014_10
- 특허 번호
- US08871945B2
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