Pyridine → HCID 13176887, 화합물

HRID 371426

반응식

HRID 371426 반응식
N1C=CC=CC=1.[CH2:7]([O:14][C:15]([NH:17][CH2:18][C:19]1[CH:27]=[CH:26][C:22]([C:23]([OH:25])=[O:24])=[CH:21][CH:20]=1)=[O:16])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C1CCC(N=C=NC2CCCCC2)CC1.CS(O[C:48]1[CH:57]=[CH:56][C:55]2[C:50](=[CH:51][CH:52]=[C:53]([C:58](=[NH:60])[NH2:59])[CH:54]=2)[CH:49]=1)(=O)=O>C(OCC)C>[CH2:7]([O:14][C:15]([NH:17][CH2:18][C:19]1[CH:20]=[CH:21][C:22]([C:23]([O:25][C:48]2[CH:57]=[CH:56][C:55]3[C:50](=[CH:51][CH:52]=[C:53]([C:58](=[NH:59])[NH2:60])[CH:54]=3)[CH:49]=2)=[O:24])=[CH:26][CH:27]=1)=[O:16])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

6

반응물 4

HCID 1049PyridineHCID 10868DicyclohexylcarbodiimideHCID 14799974-((((Benzyloxy)carbonyl)amino)methyl)benzoic acidHCID 13050560HCID 13050560, 화합물

생성물 1

HCID 13176887HCID 13176887, 화합물수율 46.9%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To 50 ml of dried pyridine, were added 5.1 g of 4-benzyloxycarbonylaminomethylbenzoic acid and 4.4 g of DCC. The mixture was stirred under cooling in ice for 30 minutes, admixed with 5.0 g of 6-amidino-2-naphthol methanesulfonate and stirred for one hour under cooling in ice, then overnight at room temperature. The reaction mixture was filtered* and the filtrate was mixed with ethyl ether. The precipitate which was formed was collected by filtration and recrystallized from a DMF-ethanol mixture to obtain 3.8 g of a white powder of a white powder of 6-amidino-2-naphthyl 4-benzyloxycarbonylaminomethylbenzoate methanesulfonate.

후처리

  1. temperatureunder cooling in ice for 30 minutes
  2. stirringstirred for one hour
  3. temperatureunder cooling in ice
  4. customovernight
  5. customat room temperature
  6. customThe precipitate which was formed
  7. filtrationwas collected by filtration
  8. customrecrystallized from a DMF-ethanol mixture

출처 및 근거

ORD 기록
ord-9e5fc2c2395f4db097b15096d444a484
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04532255

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