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Dicyclohexylcarbodiimide → HCID 17912566, 화합물

HRID 963550
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HRID 963550 반응식
C1(N=C=NC2CCCCC2)CCCCC1.[F:16][C:17]([F:25])=[CH:18][CH2:19][CH2:20][CH2:21][C:22]([OH:24])=O.[C:26]1([S:32][C:33]2[CH:39]=[CH:38][C:36]([NH2:37])=[CH:35][CH:34]=2)[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>ClCCl>[C:26]1([S:32][C:33]2[CH:39]=[CH:38][C:36]([NH:37][C:22](=[O:24])[CH2:21][CH2:20][CH2:19][CH:18]=[C:17]([F:16])[F:25])=[CH:35][CH:34]=2)[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 960814-(Phenylthio)anilineHCID 112980566,6-difluorohex-5-enoic Acid

생성물 1

HCID 17912566HCID 17912566, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

At from 0° to 10°, 20.6 g of N,N'-dicyclohexylcarbodiimide are added, while stirring, in portions to 15 g of 6,6-difluorohex-5-enoic acid in 150 ml of dichloromethane. The mixture is stirred for a further 15 minutes under cooling and then 20.1 g of 4-phenylthioaniline are added in portions. The reaction mixture is stirred for 3 hours at room temperature and then filtered. The organic phase is washed with saturated sodium hydrogen carbonate solution and then dried over sodium sulfate. After concentration by evaporation, the residue is recrystallised from toluene/hexane, yielding the title compound having a melting point of from 80° to 81° (compound no. 2-1).

후처리

  1. temperatureunder cooling
  2. stirringThe reaction mixture is stirred for 3 hours at room temperature
  3. filtrationfiltered
  4. washThe organic phase is washed with saturated sodium hydrogen carbonate solution
  5. dry with materialdried over sodium sulfate
  6. concentrationAfter concentration
  7. customby evaporation
  8. customthe residue is recrystallised from toluene/hexane

출처 및 근거

ORD 기록
ord-f99dc6f0fe7b46c4a7ab630e86f43663
출처 데이터셋
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05763481

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