Methanol → 3-Amino-5-nitropyridin-2(1H)-one
반응식
[N+:1]([C:4]1[C:5](=[O:13])[NH:6][CH:7]=[C:8]([N+:10]([O-:12])=[O:11])[CH:9]=1)([O-])=O.CO.[OH-].[NH4+].O.O.O.O.O.O.O.O.O.[S-2].[Na+].[Na+]>O>[NH2:1][C:4]1[C:5](=[O:13])[NH:6][CH:7]=[C:8]([N+:10]([O-:12])=[O:11])[CH:9]=1참가 물질
6
실험 절차
A solution of 5.5 g. of 3,5-dinitro-2-pyridone in 200 ml. of methanol was adjusted to pH 8 with ammonium hydroxide. At 60-65° C., there was added slowly a solution of 10.8 g. of sodium sulfide nonahydrate in 30 ml. of water. After 1 hour at 60-65° C. the solvent was evaporated and the residue was extracted with hot benzene and acetic acid to neutralize any sodium salt. The benzene was decanted and cooled to give a precipitate. Recrystallization from methanol gave 3-amino-5-nitro-2-pyridone, m.p. 200°-201° C.
후처리
- additionAt 60-65° C., there was added slowly a solution of 10.8 g
- customAfter 1 hour at 60-65° C. the solvent was evaporated
- extractionthe residue was extracted with hot benzene and acetic acid
- customThe benzene was decanted
- temperaturecooled
- customto give a precipitate
- customRecrystallization from methanol
출처 및 근거
- ORD 기록
- ord-2fa70162e10541fb943089f50b6b7a29
- 출처 데이터셋
- uspto-grants-1978_12
- 특허 번호
- US04131677
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