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HCID 10689660、化合物 → HCID 19353518、化合物

HRID 610836
ノート
印刷プレビュー

反応式

HRID 610836 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16]([NH:18][CH3:19])[N:15]=[C:14](Br)[CH:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[H][H]>C(O)C.[Pd]>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:13]=[CH:14][N:15]=[C:16]([NH:18][CH3:19])[CH:17]=2)(=[O:9])=[O:10])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 10689660HCID 10689660、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 19353518HCID 19353518、化合物収率 57%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

0.5 g (0.0014 mol) of 4-amino-N-(2-bromo-6-methylamino-pyridin-4-yl)-benzenesulfonamide was dissolved in 25 ml of ethanol, treated with 0.05 g of Pd/C and hydrogenated with hydrogen gas under normal pressure for 1 hour. The catalyst was filtered off, the filtrate was concentrated and the residue was dissolved in 10 ml of 1N NaOH, filtered and the filtrate was then adjusted pH 8 by means of 1N HCl. The precipitate which separated slowly was filtered off under suction, rinsed and dried in a high vacuum. There was obtained 0.22 g (57%) of 4-amino-N-(2-methylamino-pyridin-4-yl)-benzenesulfonamide as white crystals; m.p.: >261° C. (dec).

後処理

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated
  3. dissolutionthe residue was dissolved in 10 ml of 1N NaOH
  4. filtrationfiltered
  5. customThe precipitate which separated slowly
  6. filtrationwas filtered off under suction
  7. washrinsed
  8. customdried in a high vacuum

出典と根拠

ORDレコード
ord-c1f66338617f48ae8b5611d2d4295fa5
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998665

反応ノート

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