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

HRID 703668
ノート
印刷プレビュー

反応式

HRID 703668 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d9e7f4b6bca34aa7ab11a26279a49207
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04983755

反応ノート

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