反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7]([C:9]([O-:11])=O)[CH:6]=[CH:5][C:4]=1[N:12]1[CH:16]=[C:15]([CH3:17])[N:14]=[CH:13]1.[Na+].[NH:19]([C:21]([O:23][CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:22])[NH2:20].C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.C(=O)([O-])O.[Na+]>CN(C=O)C.[Cl-].[Na+].O.O>[CH3:1][O:2][C:3]1[N:8]=[C:7]([C:9]([NH:20][NH:19][C:21]([O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:22])=[O:11])[CH:6]=[CH:5][C:4]=1[N:12]1[CH:16]=[C:15]([CH3:17])[N:14]=[CH:13]1参加物
9
反応物 5
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 0 °C
実験手順
To a mixture of sodium 6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridine-2-carboxylate (12.7 g), benzyl hydrazinecarboxylate (9.10 g) and HOBt (7.4 g) in DMF (250 mL) was added WSC (8.50 g) at 0° C., and the mixture was stirred at 0° C. for 1 hr. Saturated aqueous sodium hydrogen carbonate solution (200 mL), water (400 mL) and saturated brine solution (200 mL) were added to the reaction mixture at 0° C., and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous' magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was washed with ethyl acetate and dried to give the title compound (14.6 g).
後処理
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with saturated brine
- dry with materialdried over anhydrous' magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- washThe residue was washed with ethyl acetate
- customdried
出典と根拠
- ORDレコード
- ord-eee2011ed9584e55be3b67295bb12adf
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08822699B2
関連ノート
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