反応式
[CH3:1][C:2]([CH3:7])([CH3:6])[C@H:3]([NH2:5])[CH3:4].C(N(CC)CC)C.[Cl:15][C:16]1[C:21]([C:22]2[C:27]([F:28])=[CH:26][C:25]([F:29])=[CH:24][C:23]=2[F:30])=[C:20](Cl)[N:19]2[N:32]=[CH:33][N:34]=[C:18]2[N:17]=1>ClCCl>[Cl:15][C:16]1[C:21]([C:22]2[C:23]([F:30])=[CH:24][C:25]([F:29])=[CH:26][C:27]=2[F:28])=[C:20]([NH:5][C@@H:3]([C:2]([CH3:7])([CH3:6])[CH3:1])[CH3:4])[N:19]2[N:32]=[CH:33][N:34]=[C:18]2[N:17]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
With stirring, a mixture of 1.4 mmol of (R)-3,3-dimethylbut-2-ylamine, 1.4 mmol of triethylamine and 10 ml of dichloromethane was introduced into a mixture of 1.4 mmol of 5,7-dichloro-6-(2,4,6-trifluorophenyl)-1,2,4-triazolo[1,5-a]-pyrimidine in 30 ml of dichloromethane. The reaction mixture was then stirred at room temperature for 16 hours and finally washed with 1 N hydrochloric acid and water. The organic phase was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The crude product was purified by silica gel column chromatography. This gave the title compound in the form of colorless crystals in a yield of 76% (m.p.: 169-171° C.).
後処理
- stirringThe reaction mixture was then stirred at room temperature for 16 hours
- washfinally washed with 1 N hydrochloric acid and water
- dry with materialThe organic phase was dried over anhydrous sodium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customThe crude product was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-47aeff0440d84a1f8079f3dc0a0f8a27
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06855718B2
関連ノート
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