反応式
[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]=1参加物
3
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-b01d5fb8702549929a31571549411287
- 出典データセット
- uspto-grants-1981_03
- 特許番号
- US04254122
関連ノート
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