4-Methylmorpholine → HCID 178501649, 화합물

HRID 1246215

반응식

HRID 1246215 반응식
O.ON1C2C=CC=CC=2N=N1.Cl.[CH3:13][O:14][C:15](=[O:18])[CH2:16][NH2:17].CN1CCOCC1.Cl.C(C(NCCCN(C)C)=N)C.[C:38]([C:41]1[N:42]=[C:43]([CH:46]2[CH2:54][C:53]3[C:48](=[CH:49][CH:50]=[CH:51][CH:52]=3)[N:47]2[C:55]([O:57][C:58]([CH3:61])([CH3:60])[CH3:59])=[O:56])[NH:44][CH:45]=1)(O)=[O:39]>C(Cl)Cl>[CH3:13][O:14][C:15](=[O:18])[CH2:16][NH:17][C:38]([C:41]1[N:42]=[C:43]([CH:46]2[CH2:54][C:53]3[C:48](=[CH:49][CH:50]=[CH:51][CH:52]=3)[N:47]2[C:55]([O:57][C:58]([CH3:61])([CH3:60])[CH3:59])=[O:56])[NH:44][CH:45]=1)=[O:39]

참가 물질

7

반응물 5

HCID 79724-MethylmorpholineHCID 122755Glycine methyl ester hydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 178451416HCID 178451416, 화합물HCID 178458058HCID 178458058, 화합물

생성물 1

HCID 178501649HCID 178501649, 화합물수율 69.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-Hydroxybenzotriazole hydrate (0.00036 mole), glycine methylester, hydrochloride (0.00047 mole), 4-methylmorpholine (0.00055 mole), and N′-(ethylcarbonimidoyl)-N,N-dimethyl-1,3-propanediamine monohydrochloride (0.00047 mole) were added to compound 117 (0.00036 mole) dissolved in DCM (30 ml) at 0° C. The mixture was allowed to warm to room temperature under nitrogen, and stirred overnight. The mixture was extracted with water, saturated NaHCO3, 2N citric acid, then saturated NaHCO3, dried, filtered, and concentrated, yielding 0.100 g (69%) of 1,1-dimethylethyl 2,3-dihydro-2-[4-[[(2-methoxy-2-oxoethyl)amino]carbonyl]-1H-imidazol-2-yl]-1H-indole-1-carboxylate (compound 118).

후처리

  1. extractionThe mixture was extracted with water, saturated NaHCO3, 2N citric acid
  2. dry with materialsaturated NaHCO3, dried
  3. filtrationfiltered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1838593a875e4541ab89b8c4dbf1848b
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07125891B2

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