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Hydrazinecarboxylic acid, ethyl ester → 4-Chloro-4'-methylmercaptomethylbenzophenone ethoxycarbonylhydrazone

HRID 1421542
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HRID 1421542 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][S:15][CH3:16])=[CH:10][CH:9]=2)=O)=[CH:4][CH:3]=1.[C:19]([O:23][CH2:24][CH3:25])(=[O:22])[NH:20][NH2:21]>C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.C(O)C>[CH2:24]([O:23][C:19]([NH:20][N:21]=[C:6]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][S:15][CH3:16])=[CH:10][CH:9]=1)[C:5]1[CH:17]=[CH:18][C:2]([Cl:1])=[CH:3][CH:4]=1)=[O:22])[CH3:25]
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참가 물질

5

반응물 2

HCID 20064Hydrazinecarboxylic acid, ethyl esterHCID 196893654-Chloro-4'-methylthiomethylbenzophenone

생성물 1

HCID 539729254-Chloro-4'-methylmercaptomethylbenzophenone ethoxycarbonylhydrazone수율 86.4%

시약·촉매·용매 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)촉매HCID 702Ethanol용매

실험 절차

An ethanol solution (100 ml) of 4-chloro-4'-methylmercaptomethylbenzophenone (8.3 g), ethyl carbazate (10 g) and pyridinium p-toluenesulfonate (0.1 g) was heated for 16 hours with refluxing. After cooling to a room temperature, the reaction mixture was poured into ice water, and then the precipitated crystals were collected by filtration, and washed with water. After air-drying, 4-chloro-4'-methylmercaptomethylbenzophenone ethoxycarbonylhydrazone (9.4 g) was obtained as an isomer mixture.

후처리

  1. temperaturewith refluxing
  2. filtrationthe precipitated crystals were collected by filtration
  3. washwashed with water
  4. customAfter air-drying

출처 및 근거

ORD 기록
ord-26a8f36fbe80426e8e59c2e85d55cee4
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06077866

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