Hydrazine hydrate (1:1) → 4-Chloro-N-[5-chloro-2-(4-oxo-3,4-dihydro-phthalazin-1-yl)-Pyridin-3-yl]-3-trifluoromethyl-benzenesulfonamide

HRID 1438556ノート

反応式

HRID 1438556 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:19][S:20]([C:23]2[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([C:30]([F:33])([F:32])[F:31])[CH:24]=2)(=[O:22])=[O:21])[C:5]([C:8]([C:10]2[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=2[C:12]([OH:14])=O)=O)=[N:6][CH:7]=1.O.[NH2:35][NH2:36]>C(O)C>[Cl:29][C:26]1[CH:27]=[CH:28][C:23]([S:20]([NH:19][C:4]2[C:5]([C:8]3[C:10]4[C:11](=[CH:15][CH:16]=[CH:17][CH:18]=4)[C:12](=[O:14])[NH:36][N:35]=3)=[N:6][CH:7]=[C:2]([Cl:1])[CH:3]=2)(=[O:21])=[O:22])=[CH:24][C:25]=1[C:30]([F:33])([F:32])[F:31]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 116565312-[5-Chloro-3-(4-chloro-3-trifluoromethyl-benzenesulfonylamino)-pyridine-2-carbonyl]benzoic acid

生成物 1

HCID 116349264-Chloro-N-[5-chloro-2-(4-oxo-3,4-dihydro-phthalazin-1-yl)-Pyridin-3-yl]-3-trifluoromethyl-benzenesulfonamide収率 67.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-[5-Chloro-3-(4-chloro-3-trifluoromethyl-benzenesulfonylamino)-pyridine-2-carbonyl]-benzoic acid (18 mg, 0.0347 mmol) and 2.3 mg of hydrazine hydrate in 1.0 ml of ethanol was refluxed for 4 hours. After cooled to room temperature the mixture was concentrated and the residue was purified via preparative TLC to afford 12 mg of title compound as a white powder. MS: (M+H)/z =515.2.

後処理

  1. temperaturewas refluxed for 4 hours
  2. concentrationwas concentrated
  3. customthe residue was purified via preparative TLC

出典と根拠

ORDレコード
ord-ab59dbdbbb92443da7dbc07ae27a979d
出典データセット
uspto-grants-2009_11
特許番号
US07622583B2

反応ノート

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