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Water → 1-Tert-butyl-3-(3-oxo-1-cyclohexene-1-yl)urea

HRID 1414913
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HRID 1414913 반응식
[C:1]1(=O)[CH2:6][CH2:5][CH2:4][C:3](=[O:7])[CH2:2]1.[C:9]([NH:13][C:14]([NH2:16])=[O:15])([CH3:12])([CH3:11])[CH3:10].O>C1C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>[C:9]([NH:13][C:14]([NH:16][C:1]1[CH2:6][CH2:5][CH2:4][C:3](=[O:7])[CH:2]=1)=[O:15])([CH3:12])([CH3:11])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 104341,3-CyclohexanedioneHCID 14233(1,1-Dimethylethyl)urea

생성물 1

HCID 214860551-Tert-butyl-3-(3-oxo-1-cyclohexene-1-yl)urea수율 66.7%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 241Benzene용매

실험 절차

To a solution of 11.2 g of 1,3-cyclohexanedione in 250 ml of benzene is added 11.6 g tert-butylurea and 100 mg of p-toluenesulfonic acid. The solution is heated at reflux under nitrogen with water removal for three hours. At the end of this period the solution is cooled and the precipitated product removed by filtration. The precipitate is recrystallized from acetonitrile to give 14 g of 1-tert-butyl-3-(3-oxo-1-cyclohexene-1-yl)urea, m.p. 223°-225° C.

후처리

  1. temperatureThe solution is heated
  2. temperatureAt the end of this period the solution is cooled
  3. customthe precipitated product removed by filtration
  4. customThe precipitate is recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-8431755f137a43b69ed8b570e3c7ee3b
출처 데이터셋
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04002767

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