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Water → 3-amino-N-{3-[(2-chloro-5-methoxyphenyl)amino]quinoxalin-2-yl}benzenesulfonamide hydrochloride

HRID 2201399
ノート
印刷プレビュー

反応式

HRID 2201399 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[NH:10][C:11]1[C:12]([NH:21][S:22]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([N+:31]([O-])=O)[CH:26]=2)(=[O:24])=[O:23])=[N:13][C:14]2[C:19]([N:20]=1)=[CH:18][CH:17]=[CH:16][CH:15]=2.C1COCC1.O.C([O-])=O.[K+]>[Pt]=S.CO.C(O)C>[ClH:1].[NH2:31][C:27]1[CH:26]=[C:25]([S:22]([NH:21][C:12]2[C:11]([NH:10][C:3]3[CH:4]=[C:5]([O:8][CH3:9])[CH:6]=[CH:7][C:2]=3[Cl:1])=[N:20][C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[N:13]=2)(=[O:24])=[O:23])[CH:30]=[CH:29][CH:28]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 2735122Potassium FormateHCID 57448456N-(3-((2-chloro-5-methoxyphenyl)amino)quinoxalin-2-yl)-3-nitrobenzenesulfonamide

生成物 1

HCID 894999603-amino-N-{3-[(2-chloro-5-methoxyphenyl)amino]quinoxalin-2-yl}benzenesulfonamide hydrochloride

試薬・触媒・溶媒 3

HCID 82861
Platinum sulfide (PtS)
触媒
HCID 702Ethanol溶媒
HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

To 1 kg of N-{3-[(2-chloro-5-methoxyphenyl)amino]quinoxalin-2-yl}-3-nitrobenzenesulfonamide, add a catalytic amount of platinum sulfide on carbon (Pt(S)C), 6 volumes of THF, 0.16 volume of water and 2 volumes of ethanol. The reaction mixture is stirred and heated to reflux. An aqueous potassium formate solution (1.4 volume of water+0.69 kg of potassium formate) is added. The reaction mixture is stirred at reflux until completion of the reaction and cooled down at 50° C. After the addition of 10 volumes of methanol and a one hour stirring, the catalyst is filtered off and washed with 3.4 volumes of methanol. The filtered solution is cooled down at 20° C. 0.62 kg of HCl are added. The reaction mixture is stirred at 20° C., cooled down at 5° C. and filtered. The cake is washed with methanol (6 volumes) and dried under vacuum.

後処理

  1. temperatureheated to reflux
  2. stirringThe reaction mixture is stirred
  3. temperatureat reflux until completion of the reaction
  4. stirringa one hour stirring
  5. filtrationthe catalyst is filtered off
  6. washwashed with 3.4 volumes of methanol
  7. temperatureThe filtered solution is cooled down at 20° C
  8. addition0.62 kg of HCl are added
  9. stirringThe reaction mixture is stirred at 20° C.
  10. temperaturecooled down at 5° C.
  11. filtrationfiltered
  12. washThe cake is washed with methanol (6 volumes)
  13. customdried under vacuum

出典と根拠

ORDレコード
ord-f81d3f49e3114d5daaddb3c29e9f27a3
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09364475B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート