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

HRID 605323노트

반응식

HRID 605323 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-de81cd1c60ab4523be21d9c2583348bd
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07910595B2

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