反応式
CS([O:5][CH2:6][C:7]1[CH:12]=[C:11]([C:13]([O:15][CH2:16][CH3:17])=[CH2:14])[N:10]=[C:9]([Cl:18])[N:8]=1)(=O)=O.[F:19][CH2:20][CH:21](O)[CH2:22][F:23].[OH-].[Na+]>C1C=CC=CC=1.S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC>[Cl:18][C:9]1[N:8]=[C:7]([CH2:6][O:5][CH:21]([CH2:22][F:23])[CH2:20][F:19])[CH:12]=[C:11]([C:13]([O:15][CH2:16][CH3:17])=[CH2:14])[N:10]=1参加物
6
反応物 3
生成物 1
試薬・触媒・溶媒 2
実験手順
To a solution of (2-chloro-6-(1-ethoxyvinyl)pyrimidin-4-yl)methyl methanesulfonate (0.50 g, 1.71 mmol) in benzene (10 mL), was added 1,3-difluoro-2-propanol (0.246 g, 2.56 mmol). Sodium hydroxide (5M (aq), 0.512 mL, 2.56 mmol) and tetrabutylammonium hydrogen sulfate (0.058 g, 0.17 mmol) were added. The mixture was stirred vigorously at rt over night. The mixture was filtered through a short silica plug with magnesium sulfate. The filter plug was eluted with EtOAc and the solvents were evaporated. The residue was purified by preparative HPLC to give the title compound as a solid (0.054 g, 11%).
後処理
- filtrationThe mixture was filtered through a short silica plug with magnesium sulfate
- washThe filter plug was eluted with EtOAc
- customthe solvents were evaporated
- customThe residue was purified by preparative HPLC
出典と根拠
- ORDレコード
- ord-4c6906f8869b4deab1d78f128dc10bbd
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09439904B2
関連ノート
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