m-Toluohydrazide → HCID 136359954、化合物

HRID 1019442

反応式

HRID 1019442 の反応式
[Cl:1][C:2]1[C:3]([OH:10])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=O.[CH3:11][C:12]1[CH:13]=[C:14]([CH:19]=[CH:20][CH:21]=1)[C:15]([NH:17][NH2:18])=[O:16]>C(O)C>[Cl:1][C:2]1[C:3]([OH:10])=[C:4]([CH:5]=[N:18][NH:17][C:15](=[O:16])[C:14]2[CH:19]=[CH:20][CH:21]=[C:12]([CH3:11])[CH:13]=2)[CH:7]=[CH:8][CH:9]=1

参加物

4

反応物 2

HCID 83082m-ToluohydrazideHCID 5196513-Chloro-2-hydroxybenzaldehyde

生成物 1

HCID 136359954HCID 136359954、化合物収率 25%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

A suspension of 3-chloro-2-hydroxy-benzaldehyde (0.100 g, 0.639 mmol) and 3-methyl-benzoic acid hydrazide (0.096 g, 0.639 mmol) in ethanol (2 mL) was heated to 60° C. for 18 hours. The reaction mixture was cooled to room temperature to precipitate the product. The solid was collected via suction filtration and rinsed with ethanol to furnish 3-methyl-benzoic acid [1-(3-chloro-2-hydroxy-phenyl)-methylidene]-hydrazide as a white solid (0.046 g, 25%): mp 166-169° C.; 1H NMR (400 MHz, CDCl3) δ 8.59 (d, J=12.0 Hz, 1H), 7.76 (d, J=10.0 Hz, 2H), 7.47 (dd, J=15.6, 6.2 Hz, 4H), 6.97 (t, J=7.8 Hz, 1H), 2.39 (d, J=12.0 Hz, 3H); ESIMS m/z 289 ([M+H]+), 287 ([M−H]−).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customto precipitate the product
  3. filtrationThe solid was collected via suction filtration
  4. washrinsed with ethanol

出典と根拠

ORDレコード
ord-9b3d0a7bc62b4062b720883f8e3fb3ad
出典データセット
uspto-grants-2014_05
特許番号
US08715745B2

関連ノート

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