Water → HCID 178470174, 화합물

HRID 1595315노트

반응식

HRID 1595315 반응식
O[N:2]=[C:3]([C:9]([C:11]1[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][CH:12]=1)=O)[C:4]([O:6][CH2:7][CH3:8])=[O:5].[C:18]1([CH2:28][NH2:29])[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:21]=[CH:20][CH:19]=1.O>C1(C)C(C)=CC=CC=1>[CH3:17][C:14]1[CH:15]=[CH:16][C:11]([C:9]2[NH:29][C:28]([C:18]3[C:27]4[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=4)[CH:21]=[CH:20][CH:19]=3)=[N:2][C:3]=2[C:4]([O:6][CH2:7][CH3:8])=[O:5])=[CH:12][CH:13]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 83551-NaphthalenemethanamineHCID 178472891HCID 178472891, 화합물

생성물 1

HCID 178470174HCID 178470174, 화합물수율 12%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

Ethyl 2-hydroxyimino-3-(4-methylphenyl)-3-oxopropionate (13.7 g) and 1-naphthalenemethylamine (11.0 g) were dissolved in xylene (137 ml), andrefluxed underheating for 9 hr whiledehydrating with Dean-stark trap. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and dried. The solvent was concentrated under reduced pressure and isopropyl alcohol was added to the obtained residue to allow crystallization. The crystals were collected by filtration to give ethyl 5-(4-methylphenyl)-2-(1-naphthyl)-imidazole-4-carboxylate (2.5 g), melting point 190-192° C.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. customdried
  4. concentrationThe solvent was concentrated under reduced pressure and isopropyl alcohol
  5. additionwas added to the obtained residue
  6. customcrystallization
  7. filtrationThe crystals were collected by filtration

출처 및 근거

ORD 기록
ord-cbbbe388db8b49608e8aa613f70d0897
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06288061B1

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