反応式
Cl[C:2]1[C:7]([O:8][CH3:9])=[C:6]([Cl:10])[N:5]=[CH:4][N:3]=1.[CH3:11][C:12]([CH3:32])([CH3:31])[CH2:13][C:14]1[N:19]=[C:18]([CH2:20][OH:21])[CH:17]=[CH:16][C:15]=1[C:22]1[CH:27]=[C:26]([O:28][CH3:29])[CH:25]=[CH:24][C:23]=1[F:30].[H-].[Na+].Cl>C1COCC1>[Cl:10][C:6]1[C:7]([O:8][CH3:9])=[C:2]([O:21][CH2:20][C:18]2[CH:17]=[CH:16][C:15]([C:22]3[CH:27]=[C:26]([O:28][CH3:29])[CH:25]=[CH:24][C:23]=3[F:30])=[C:14]([CH2:13][C:12]([CH3:32])([CH3:31])[CH3:11])[N:19]=2)[N:3]=[CH:4][N:5]=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
- 50 °C
実験手順
To a solution of 4,6-dichloro-5-methoxypyrimidine (450 mg) and (6-(2,2-dimethylpropyl)-5-(2-fluoro-5-methoxyphenyl)pyridin-2-yl)methanol (760 mg) in THF (8.0 mL) was added 60% sodium hydride (200 mg) at 0° C., and the mixture was stirred at 50° C. for 2 hr. The reaction mixture was neutralized with 1N hydrochloric acid, and extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (1.05 g) as a white solid.
後処理
- extractionextracted with ethyl acetate
- washThe extract was washed with saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-509e63ab996b4640a72d67164b916ff6
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09181186B2
関連ノート
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