반응식
C([N:4](CC)C(C)C)(C)C.O.NN.Cl.[N+:14]([C:17]1[CH:22]=[CH:21][C:20]([C:23](=[NH:25])[NH2:24])=[CH:19][CH:18]=1)([O-:16])=[O:15].[Cl-].[Na+]>CO.C(OCC)(=O)C>[N+:14]([C:17]1[CH:18]=[CH:19][C:20]([C:23](=[NH:24])[NH:25][NH2:4])=[CH:21][CH:22]=1)([O-:16])=[O:15]참가 물질
7
실험 절차
At 0° C., 5.2 ml (29.8 mmol, 3 eq.) of N,N-diisopropylethylamine and 0.62 g (purity 80%, 9.92 mmol, 1.0 eq.) of hydrazine monohydrate were added to a solution of 2.0 g (9.92 mmol) of 4-nitrobenzenecarboximidamide monohydrochloride in 20 ml of methanol, and the mixture was stirred at RT for 64 h. The reaction mixture was then added to 10% strength sodium chloride solution and, after addition of ethyl acetate and phase separation, was extracted twice with ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated under reduced pressure. Yield: 1.7 g (93% of theory)
후처리
- extractionwas extracted twice with ethyl acetate
- dry with materialThe combined organic phases were dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-05d02b578f3241d1adb7583028d7eb0a
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09434690B2
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