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1,2-Dichloroethane → 4-(5-{3-[3-Ethyl-3-(3-hydroxy-phenyl)-azepan-1-yl]-3-oxo-propyl}-imidazol-1-ylmethyl)-2-fluoro-benzonitrile

HRID 429070
ノート
印刷プレビュー

反応式

HRID 429070 の反応式
[C:1]([C:3]1[CH:19]=[CH:18][C:6]([CH2:7][N:8]2[C:12]([CH2:13][CH2:14][C:15]([OH:17])=O)=[CH:11][N:10]=[CH:9]2)=[CH:5][C:4]=1[F:20])#[N:2].[CH2:21]([C:23]1([C:30]2[CH:31]=[C:32]([OH:36])[CH:33]=[CH:34][CH:35]=2)[CH2:29][CH2:28][CH2:27][CH2:26][NH:25][CH2:24]1)[CH3:22].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.CN1CCOCC1>CN(C=O)C>[CH2:21]([C:23]1([C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([OH:36])[CH:31]=2)[CH2:29][CH2:28][CH2:27][CH2:26][N:25]([C:15](=[O:17])[CH2:14][CH2:13][C:12]2[N:8]([CH2:7][C:6]3[CH:18]=[CH:19][C:3]([C:1]#[N:2])=[C:4]([F:20])[CH:5]=3)[CH:9]=[N:10][CH:11]=2)[CH2:24]1)[CH3:22]
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 757711-HydroxybenzotriazoleHCID 6453793N-DesmethylmeptazinolHCID 183543083-[3-(4-cyano-3-fluoro-benzyl)-3H-imidazol-4-yl]-propionic Acid

生成物 1

HCID 183543074-(5-{3-[3-Ethyl-3-(3-hydroxy-phenyl)-azepan-1-yl]-3-oxo-propyl}-imidazol-1-ylmethyl)-2-fluoro-benzonitrile

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3-[3-(4-Cyano-3-fluoro-benzyl)-3H-imidazol-4-yl]-propionic acid, as described above in Step E, (0.56 g, 0.78 mmol) and 3-(3-ethyl-azepan-3-yl)-phenol, as described above in Step J, (0.182 g, 0.78 mmol), HOBT (0.126 g, 0.936 mmol), EDC (0.179 g, 0.936 mmol) and N-methylmorpholine (0.257 mL, 2.34 mmol) were dissolved in DMF (15 mL) and stirred at ambient temperature for 18 h. The DMF was removed in vacuo and the residue was partitioned between EtOAc and saturated aqueous NaHCO3 solution. The organic layer was washed with H2O, brine, dried (MgSO4), filtered, and concentrated to give the title compound.

後処理

  1. customThe DMF was removed in vacuo
  2. customthe residue was partitioned between EtOAc and saturated aqueous NaHCO3 solution
  3. washThe organic layer was washed with H2O, brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-0e5f9eacc7174d699880c1ba3186aea6
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06316436B1

反応ノート

読み込み中…

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