반응식
[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]1참가 물질
9
반응물 5
생성물 1
시약·촉매·용매 3
반응 조건
- 온도
- 0 °C
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-eee2011ed9584e55be3b67295bb12adf
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08822699B2
연결된 노트
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