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1,2-Dichloroethane → {2-[1-(4-Cyano-3-fluoro-phenyl)-1-(3-methyl-3H-imidazol-4-yl)-ethylcarbamoyl]-ethyl}-carbamic acid

HRID 1060884
ノート
印刷プレビュー

反応式

HRID 1060884 の反応式
C([O:5][C:6]([NH:8][CH2:9][CH2:10][C:11]([OH:13])=O)=[O:7])(C)(C)C.N1C2C(=NC=CC=2)N(O)N=1.C(Cl)CCl.CN1CCOCC1.[NH2:35][C:36]([C:44]1[CH:51]=[CH:50][C:47]([C:48]#[N:49])=[C:46]([F:52])[CH:45]=1)([C:38]1[N:39]([CH3:43])[CH:40]=[N:41][CH:42]=1)[CH3:37]>CN(C=O)C>[C:48]([C:47]1[CH:50]=[CH:51][C:44]([C:36]([NH:35][C:11]([CH2:10][CH2:9][NH:8][C:6](=[O:7])[OH:5])=[O:13])([C:38]2[N:39]([CH3:43])[CH:40]=[N:41][CH:42]=2)[CH3:37])=[CH:45][C:46]=1[F:52])#[N:49]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 76809N-((1,1-dimethylethoxy)carbonyl)-beta-alanineHCID 181649HOAtHCID 11470581(+)-4-[1-amino-1-(3-methyl-3H-imidazol-4-yl)-ethyl]-2-fluoro-benzonitrile

生成物 1

HCID 70025288{2-[1-(4-Cyano-3-fluoro-phenyl)-1-(3-methyl-3H-imidazol-4-yl)-ethylcarbamoyl]-ethyl}-carbamic acid

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 3-tert-butoxycarbonylamino-propionic acid (0.77 g, 4.09 mmol) in DMF (8.2 mL) at ambient temperature was added [1,2,3]triazolo[4,5-b]pyridin-3-ol (HOAT) (0.53 g, 3.89 mmol), EDC (0.82 g, 4.30 mmol), and 4-methylmorpholine (0.41 g, 4.09 mmol), followed by (+)-4-[1-amino-1-(3-methyl-3H-imidazol-4-yl)-ethyl]-2-fluoro-benzonitrile (Example 1, Step I) (1.00 g, 4.09 mmol). After stirring overnight, the reaction was concentrated in vacuo to remove the DMF. The residue was partitioned between EtOAc and saturated aqueous NaHCO3 solution, the organic layer washed with brine, dried (Na2SO4), and concentrated in vacuo to provide the crude title compound.

後処理

  1. concentrationthe reaction was concentrated in vacuo
  2. customto remove the DMF
  3. customThe residue was partitioned between EtOAc and saturated aqueous NaHCO3 solution
  4. washthe organic layer washed with brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-97dadc4a13ae421fa9725a7fbfe48654
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06525074B2

反応ノート

読み込み中…

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