反応式
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:4]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]([NH2:20])=[O:19])=[C:13]3[NH:12][CH2:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1.C(=O)=O.CC(C)=O.[H-].[Na+].[C:32](N1C=CN=C1)(N1C=CN=C1)=[S:33]>O1CCCC1>[S:33]=[C:32]1[N:12]2[C:13]3[N:14]([C:9]([C:5]4[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:21])([F:1])[F:22])[CH:4]=4)=[CH:10][CH2:11]2)[N:15]=[CH:16][C:17]=3[C:18](=[O:19])[NH:20]1参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- -78 °C
実験手順
To a stirred solution of 1.00 g of 4,5-dihydro-7-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carboxamide (prepared as described in Example 4) in 30 ml of dry tetrahydrofuran cooled to -78° C. (dry ice-acetone) was added 286 mg of 60% sodium hydride (dispersion in mineral oil). The reaction mixture was stirred at -78° C. for 30 minutes then 637 mg of 1,1'-thiocarbonyldiimidazole was added. The mixture was allowed to slowly warm to room temperature and was stirred for 36 hours. The reaction mixture was quenched with water, neutralized with 5% aqueous hydrochloric acid and extracted with chloroform. Evaporation of the solvent in vacuo gave 934 mg of the desired product as a yellow solid, m.p. 251°-258° C. (dec).
後処理
- temperatureto slowly warm to room temperature
- stirringwas stirred for 36 hours
- customThe reaction mixture was quenched with water
- extractionextracted with chloroform
- customEvaporation of the solvent in vacuo
出典と根拠
- ORDレコード
- ord-65257aa5722d492ab3d7ec7361c0fd72
- 出典データセット
- uspto-grants-1990_04
- 特許番号
- US04916137
関連ノート
読み込み中…