4-Methylmorpholine → HCID 178501649、化合物

HRID 887936

反応式

HRID 887936 の反応式
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]

参加物

7

反応物 5

HCID 79724-MethylmorpholineHCID 122755Glycine methyl ester hydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 178451416HCID 178451416、化合物HCID 178458058HCID 178458058、化合物

生成物 1

HCID 178501649HCID 178501649、化合物収率 69.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-b658bee3c3c147aebd5bce6d7e7f4a21
出典データセット
uspto-grants-2012_08
特許番号
US08247432B2

関連ノート

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