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Ethyl chloroformate → HCID 53960004, 화합물

HRID 1448345
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HRID 1448345 반응식
[CH3:1][O:2][CH2:3][C:4]1([NH:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:9][CH2:8][N:7]([C:10]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[O:11])[CH2:6][CH2:5]1.[C:27](Cl)(=[O:31])[O:28][CH2:29][CH3:30]>>[CH2:29]([O:28][C:27]([N:20]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:4]1([CH2:3][O:2][CH3:1])[CH2:5][CH2:6][N:7]([C:10]([O:12][CH2:13][C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)=[O:11])[CH2:8][CH2:9]1)=[O:31])[CH3:30]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 10928Ethyl chloroformateHCID 54398456HCID 54398456, 화합물

생성물 1

HCID 53960004HCID 53960004, 화합물수율 83.5%

반응 조건

온도
110 °C

실험 절차

A mixture of 14.2 parts of (phenylmethyl) 4-(methoxymethyl)-4-(phenylamino)-1-piperidinecarboxylate and 170.2 parts of ethyl carbonochloridate is stirred and refluxed for 16 hours in an oil-bath at 110° C. The reaction mixture is evaporated and the residue is dissolved in 225 parts of trichloromethane. The solution is washed twice with water, dried, filtered and evaporated. The residue is dissolved in methylbenzene and the latter is evaporated again, yielding 14.2 parts (83.5%) of (phenylmethyl) 4-[(ethoxycarbonyl)phenylamino]-4-(methoxymethyl)-1-piperidinecarboxylate as a residue.

후처리

  • customThe reaction mixture is evaporated
  • dissolutionthe residue is dissolved in 225 parts of trichloromethane
  • washThe solution is washed twice with water
  • customdried
  • filtrationfiltered
  • customevaporated
  • dissolutionThe residue is dissolved in methylbenzene
  • customthe latter is evaporated again
  • 출처 및 근거

    ORD 기록
    ord-752c8b67c2f04f4d9e1be26327f969fc
    출처 데이터셋
    uspto-grants-1979_12
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04179569

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