Water → 4-(4-Amino-phenylsulfanyl)-N-(5-bromo-pyridin-2-yl)-3-nitro-benzamide

HRID 605323ノート

反応式

HRID 605323 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9](=[O:20])[C:10]2[CH:15]=[CH:14][C:13](Cl)=[C:12]([N+:17]([O-:19])=[O:18])[CH:11]=2)=[N:6][CH:7]=1.[NH2:21][C:22]1[CH:27]=[CH:26][C:25]([SH:28])=[CH:24][CH:23]=1.O.O.O.C([O-])(=O)C.[Na+].O>C(O)C>[NH2:21][C:22]1[CH:27]=[CH:26][C:25]([S:28][C:13]2[CH:14]=[CH:15][C:10]([C:9]([NH:8][C:5]3[CH:4]=[CH:3][C:2]([Br:1])=[CH:7][N:6]=3)=[O:20])=[CH:11][C:12]=2[N+:17]([O-:19])=[O:18])=[CH:24][CH:23]=1

参加物

6

反応物 4

HCID 962WaterHCID 145104-AminothiophenolHCID 5023018N-(5-bromopyridin-2-yl)-4-chloro-3-nitrobenzamideHCID 23665404Sodium Acetate Trihydrate

生成物 1

HCID 670400914-(4-Amino-phenylsulfanyl)-N-(5-bromo-pyridin-2-yl)-3-nitro-benzamide収率 99%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of the product of Example 364A (24.2 g, 0.0678 mol), 4-amino-benzenethiol (12.7 g, 0.102 mol, 1.5 equiv.), and sodium acetate trihydrate (46.1 g, 0.339 mol, 5.0 equiv.) in 500 mL of ethanol was heated under reflux under nitrogen with stirring for 2 hours. The reaction mixture was then allowed to cool to room temperature and 200 mL of water added. The mixture was stirred for 30 minutes, filtered, and dried in vacuo to give the title compound (29.8 g, 99%).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux under nitrogen
  3. stirringThe mixture was stirred for 30 minutes
  4. filtrationfiltered
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-de81cd1c60ab4523be21d9c2583348bd
出典データセット
uspto-grants-2011_03
特許番号
US07910595B2

反応ノート

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