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Dicyclohexylcarbodiimide → HCID 69941397, 화합물

HRID 324154
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HRID 324154 반응식
[CH3:1][C@H:2]([C:11]([O:13][C:14]1[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=1)=[O:12])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[CH2:21]([O:28][C:29]1[CH:37]=[CH:36][C:32]([C:33](O)=[O:34])=[CH:31][CH:30]=1)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C1CCC(N=C=NC2CCCCC2)CC1>ClCCl>[CH3:1][C@H:2]([C:11]([O:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][C:33]([C:32]2[CH:36]=[CH:37][C:29]([O:28][CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[CH:30][CH:31]=2)=[O:34])=[CH:16][CH:15]=1)=[O:12])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 738804-(Benzyloxy)benzoic acidHCID 20645780HCID 20645780, 화합물

생성물 1

HCID 69941397HCID 69941397, 화합물수율 68.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

{circle around (3)}: A mixture comprising 1.66 g of (S)-4-(1′-methylnonylcarbonyloxy)phenol, 1.37 g of 4-benzyloxybenzoic acid, 1.24 g of DCC and 10 g of dichloromethane was stirred at room temperature for 30 minutes. Then, a catalytic amount of 4-N,N-dimethylaminopyridine was added to the mixture, and the mixture was further stirred at room temperature for 12 hours. After finishing the reaction, insoluble substances were filtered off, followed by distilling off dichloromethane from the filtrate under reduced pressure. The resultant residue was purified by means of silica gel column chromatography, whereby 2.0 g of (S)-4-[4′-(1″-methylnonylcarbonyloxy)phenyloxycarbonyl]-1-benzyloxybenzene was obtained in the form of a colorless crystal.

후처리

  1. stirringthe mixture was further stirred at room temperature for 12 hours
  2. customthe reaction, insoluble substances
  3. filtrationwere filtered off
  4. distillationby distilling off dichloromethane from the filtrate under reduced pressure
  5. customThe resultant residue was purified by means of silica gel column chromatography

출처 및 근거

ORD 기록
ord-f1c78c18e21047358824379b5d8ec131
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06217793B1

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