Ethanone, 1-(2,5-dichlorophenyl)- → N'-[(1E)-1-(2,5-Dichlorophenyl)ethylidene]-3-(morpholine-4-sulfonyl)benzohydrazide

HRID 877604

反応式

HRID 877604 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[C:9](=O)[CH3:10].[O:12]1[CH2:17][CH2:16][N:15]([S:18]([C:21]2[CH:22]=[C:23]([CH:28]=[CH:29][CH:30]=2)[C:24]([NH:26][NH2:27])=[O:25])(=[O:20])=[O:19])[CH2:14][CH2:13]1>CO.C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1/[C:9](=[N:27]/[NH:26][C:24](=[O:25])[C:23]1[CH:28]=[CH:29][CH:30]=[C:21]([S:18]([N:15]2[CH2:16][CH2:17][O:12][CH2:13][CH2:14]2)(=[O:19])=[O:20])[CH:22]=1)/[CH3:10]

参加物

5

反応物 2

HCID 75587Ethanone, 1-(2,5-dichlorophenyl)-HCID 8772463-(Morpholine-4-sulfonyl)benzohydrazide

生成物 1

HCID 9606714N'-[(1E)-1-(2,5-Dichlorophenyl)ethylidene]-3-(morpholine-4-sulfonyl)benzohydrazide

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 887Methanol溶媒

反応条件

温度
120 °C

実験手順

1-(2,5-Dichlorophenyl)ethanone (20 mg, 0.106 mmol) and 3-(morpholinosulfonyl)benzohydrazide (30.2 mg, 0.106 mmol) were dissolved in methanol (4 mL) in the presence of acetic acid as a catalyst, and the reaction mixture was heated via microwave irradiation to 120° C. for 30 min. Following cooling, the solvent was removed by vacuum and the resulting crude material was purified by flash column chromatography affording the title compound in a 10 mg yield. 1H NMR (400 MHz, CDCl3): δ 8.29 (m, 1H), 8.09 (m, 1H), 7.81 (m, 1H), 7.57 (m, 1H), 7.40 (m, 1H), 7.26 (m, 2H), 3.52 (m, 4H), 2.91 (m, 4H), 2.28 (s, 3H). ESI-MS: 456.1 [M+H]+.

後処理

  1. temperatureFollowing cooling
  2. customthe solvent was removed by vacuum
  3. customthe resulting crude material was purified by flash column chromatography

出典と根拠

ORDレコード
ord-430ecb90955b4d0f9e6885f78cb8e5fb
出典データセット
uspto-grants-2015_03
特許番号
US08987335B2

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