Sodium Hydroxide → HCID 178503121, 화합물

HRID 1435583노트

반응식

HRID 1435583 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]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 832304-(Methylthio)benzoic acidHCID 34801515-Nitropyridine-2,3-diamine

생성물 1

HCID 178503121HCID 178503121, 화합물

시약·촉매·용매 1

HCID 962Water용매

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. Yield 0.656 g of 30% purity

후처리

  1. temperatureThe mixture was cooled
  2. filtrationthe precipitate collected by filtration
  3. stirringThe filtration residue was stirred in 50 ml pyridine at 60° C.
  4. temperaturecooled
  5. custominsoluble components removed by filtration
  6. customThe filtrate was evaporated
  7. customthe residue used without further purification in the next steps

출처 및 근거

ORD 기록
ord-c68eca9ffc4d4fcdac1cbd35637b3f5b
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618964B2

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