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

HRID 335464

반응식

HRID 335464 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-cd240b7a84414d0a9629b9b3cbb75b72
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08884010B2

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