反応式
[CH2:1]([NH2:5])[CH2:2][CH2:3][CH3:4].[F:6][C:7]([F:25])([F:24])[C:8]1[CH:9]=[C:10]([N:14]2[C:19](=[O:20])[NH:18][CH:17](SC)[NH:16][C:15]2=[O:23])[CH:11]=[CH:12][CH:13]=1>C(O)(=O)C>[F:6][C:7]([F:25])([F:24])[C:8]1[CH:9]=[C:10]([N:14]2[C:19](=[O:20])[NH:18][CH:17]([NH:5][CH2:1][CH2:2][CH2:3][CH3:4])[NH:16][C:15]2=[O:23])[CH:11]=[CH:12][CH:13]=1参加物
反応条件
- 温度
- 145 °C
実験手順
n-Butylamine (3.92 ml.) was added during 15 minutes to stirred acetic acid (2.4 ml.). After 30 minutes at room temperature, 3-(3-trifluoromethylphenyl)-6-methylthio-tetrahydro-1,3,5-triazine-2,4-dione (6.1 g.) was added to the acetic acid solution. The mixture obtained was then heated at 145° C., for 4 hours. (The liberated methylmercaptan was absorbed into a trap containing an excess of aqueous sodium hydroxide and sodium hypochlorite.) The reaction mixture was cooled to room temperature and then water (75 ml.) was added. The mixture was then stirred for 15 minutes and the white solid which formed was separated by filtration, washed with water (3×150 ml.), and dried (over phosphorus pentoxide) to give 3-(3-trifluoromethylphenyl)-6-n-butylamino-tetrahydro-1,3,5-triazine-2,4-dione (6.0 g., 95%), m.p. 245°-247° C.
後処理
- customThe mixture obtained
- custom(The liberated methylmercaptan was absorbed into a trap
- additioncontaining an excess of aqueous sodium hydroxide and sodium hypochlorite
- temperature) The reaction mixture was cooled to room temperature
- additionwater (75 ml.) was added
- customthe white solid which formed
- customwas separated by filtration
- washwashed with water (3×150 ml.)
- dry with materialdried (over phosphorus pentoxide)
出典と根拠
- ORDレコード
- ord-9490e7a2fd5c4ac0930df0f2154a72ac
- 出典データセット
- uspto-grants-1981_03
- 特許番号
- US04254122
関連ノート
読み込み中…