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Sulfuric Acid → Ethyl 3-[1-(4-chlorophenyl)-2,2-dimethylpropylidene]carbazate

HRID 703668
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반응식

HRID 703668 반응식
[C:1]([C:5]([C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1)=O)([CH3:4])([CH3:3])[CH3:2].[C:14]([O:18][CH2:19][CH3:20])(=[O:17])[NH:15][NH2:16].S(=O)(=O)(O)O>C(O)C>[Cl:13][C:10]1[CH:11]=[CH:12][C:7]([C:5](=[N:16][NH:15][C:14]([O:18][CH2:19][CH3:20])=[O:17])[C:1]([CH3:4])([CH3:3])[CH3:2])=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 20064Hydrazinecarboxylic acid, ethyl esterHCID 111380501-(4-Chlorophenyl)-2,2-dimethylpropan-1-one

생성물 1

HCID 53994370Ethyl 3-[1-(4-chlorophenyl)-2,2-dimethylpropylidene]carbazate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 4.92 g (0.025 mol) 4-chlorphenyl tert.-butyl ketone and 8.05 g (0.075 mol) ethyl carbazate in 125 ml absolute ethanol was treated with ca. 0.3 g concentrated sulphuric acid and heated at reflux for 3 hours. The solution was then concentrated in vacuo and the residue added to water. It was then extracted with ethyl acetate, the organic phase dried with magnesium sulphate, concentrated and the residue recrystallised from diisopropyl ether.

후처리

  1. temperatureheated
  2. temperatureat reflux for 3 hours
  3. concentrationThe solution was then concentrated in vacuo
  4. additionthe residue added to water
  5. extractionIt was then extracted with ethyl acetate
  6. dry with materialthe organic phase dried with magnesium sulphate
  7. concentrationconcentrated
  8. customthe residue recrystallised from diisopropyl ether

출처 및 근거

ORD 기록
ord-d9e7f4b6bca34aa7ab11a26279a49207
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04983755

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