Toluene → 2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetohydrazide

HRID 335464

反応式

HRID 335464 の反応式
[CH2:1]([C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH2:10][CH3:11])[C:4]=1[C:12](=[O:18])[C:13](OCC)=[O:14])[CH3:2].C1(C)C=CC=CC=1.O.[NH2:27][NH2:28]>O>[CH2:1]([C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH2:10][CH3:11])[C:4]=1[C:12](=[O:18])[C:13]([NH:27][NH2:28])=[O:14])[CH3:2]

参加物

5

反応物 3

HCID 1140TolueneHCID 24654Hydrazine hydrate (1:1)HCID 56942718Ethyl (2,6-diethyl-4-methylphenyl)glyoxylate

生成物 1

HCID 569428732-(2,6-Diethyl-4-methylphenyl)-2-oxoacetohydrazide

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

To a 100 mL volume three-necked flask, ethyl 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetate ((9-a) (10.0 g)) and toluene (35 ml) were added. Hydrazine hydrate (2.13 ml) was added dropwise thereto at 60° C. and the obtained mixture was stirred at 70° C. for 7 hours. The reaction mixture was cooled to room temperature, water was added thereto and the organic layer was removed. The aqueous layer was extracted with toluene. The organic layers were combined and concentrated under reduced pressure to give 9.40 g of 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetohydrazide ((12-1)-(11)-39).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customthe organic layer was removed
  3. extractionThe aqueous layer was extracted with toluene
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-cd240b7a84414d0a9629b9b3cbb75b72
出典データセット
uspto-grants-2014_11
特許番号
US08884010B2

関連ノート

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