반응식
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1.[CH3:12][S:13][C:14]1[CH:22]=[CH:21][C:17]([C:18](O)=O)=[CH:16][CH:15]=1.[OH-].[Na+]>O>[CH3:12][S:13][C:14]1[CH:22]=[CH:21][C:17]([C:18]2[NH:1][C:2]3=[N:3][CH:4]=[C:5]([N+:9]([O-:11])=[O:10])[CH:6]=[C:7]3[N:8]=2)=[CH:16][CH:15]=1참가 물질
5
실험 절차
1.0 g 2,3-diamino-5-nitropyridine and 1.125 g 4-methylsulfanylbenzoic acid in 20 ml polyphosphoric acid were heated to 160° C. with stirring for 15 hrs. The mixture was cooled and poured into water. The pH was adjusted to 4-5 by addition of sodium hydroxide and the precipitate collected by filtration. The filtration residue was stirred in 50 ml pyridine at 60° C., cooled and insoluble components removed by filtration. The filtrate was evaporated and the residue used without further purification in the next steps.
후처리
- temperatureThe mixture was cooled
- filtrationthe precipitate collected by filtration
- stirringThe filtration residue was stirred in 50 ml pyridine at 60° C.
- temperaturecooled
- custominsoluble components removed by filtration
- customThe filtrate was evaporated
- customthe residue used without further purification in the next steps
출처 및 근거
- ORD 기록
- ord-8474e7643ba740139fd5909dc95249b9
- 출처 데이터셋
- uspto-grants-2010_08
- 특허 번호
- US07786113B2
연결된 노트
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