반응식
[F:1][C:2]([F:23])([F:22])[C:3]1[CH:4]=[C:5]([N:9]2[C:14](=[O:15])[NH:13][CH:12]([NH:16][CH2:17][CH2:18][CH2:19][CH3:20])[NH:11][C:10]2=[O:21])[CH:6]=[CH:7][CH:8]=1.[C:24](OC(=O)C)(=[O:26])[CH3:25]>>[F:23][C:2]([F:22])([F:1])[C:3]1[CH:4]=[C:5]([N:9]2[C:14](=[O:15])[NH:13][CH:12]([N:16]([CH2:17][CH2:18][CH2:19][CH3:20])[C:24](=[O:26])[CH3:25])[NH:11][C:10]2=[O:21])[CH:6]=[CH:7][CH:8]=1참가 물질
3
실험 절차
A mixture of 3-(3-trifluoromethylphenyl)-6-n-butylaminotetrahydro-1,3,5-triazine-2,4-dione (4.0 g.) and acetic anhydride (40 ml.) was heated under reflux for 2 hours. The mixture was then distilled at atmospheric pressure over 2 hours, fresh acetic anhydride being added to maintain the original volume. The mixture was then distilled at atmospheric pressure so that the final volume was about 10 ml. Ether (60 ml.) and petroleum ether (b.p. 40°-60° C.) [hereinafter referred to as "40-60 petrol"] (20 ml.) was then added. The white solid which precipitated was washed with ether (2×30 ml.) and air dried to give 3-(3-trifluoromethylphenyl)-6-[(N-acetyl)-n-butylamino]-tetrahydro-1,3,5-triazine-2,4-dione (3.7 g., 66%), m.p. 146°-148° C.
후처리
- temperaturewas heated
- temperatureunder reflux for 2 hours
- distillationThe mixture was then distilled at atmospheric pressure over 2 hours
- additionfresh acetic anhydride being added
- temperatureto maintain the original volume
- distillationThe mixture was then distilled at atmospheric pressure so that the final volume
- additionwas then added
- customThe white solid which precipitated
- washwas washed with ether (2×30 ml.) and air
- customdried
출처 및 근거
- ORD 기록
- ord-b01d5fb8702549929a31571549411287
- 출처 데이터셋
- uspto-grants-1981_03
- 특허 번호
- US04254122
연결된 노트
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