Pyridine → HCID 13176887、化合物

HRID 371426

反応式

HRID 371426 の反応式
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

参加物

6

反応物 4

HCID 1049PyridineHCID 10868DicyclohexylcarbodiimideHCID 14799974-((((Benzyloxy)carbonyl)amino)methyl)benzoic acidHCID 13050560HCID 13050560、化合物

生成物 1

HCID 13176887HCID 13176887、化合物収率 46.9%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9e5fc2c2395f4db097b15096d444a484
出典データセット
uspto-grants-1985_07
特許番号
US04532255

関連ノート

読み込み中…