Sodium Hydroxide → HCID 178503121、化合物

HRID 1435583

反応式

HRID 1435583 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 178503121HCID 178503121、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-c68eca9ffc4d4fcdac1cbd35637b3f5b
出典データセット
uspto-grants-2009_11
特許番号
US07618964B2

関連ノート

読み込み中…