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Triethylamine → {2-[3-(4-cyano-3-fluoro-benzyl)-2-methyl-3H-imidazol-4-yl]-ethyl}-tert-butyl Urea

HRID 1594894
ノート
印刷プレビュー

反応式

HRID 1594894 の反応式
Cl.Cl.N[CH2:4][CH2:5][C:6]1[N:10]([CH2:11][C:12]2[CH:19]=[CH:18][C:15]([C:16]#[N:17])=[C:14]([F:20])[CH:13]=2)[C:9]([CH3:21])=[N:8][CH:7]=1.CC[N:24](CC)CC.[C:29]([N:33]=[C:34]=[O:35])([CH3:32])([CH3:31])[CH3:30]>CN(C=O)C>[C:16]([C:15]1[CH:18]=[CH:19][C:12]([CH2:11][N:10]2[C:6]([CH2:5][CH2:4][N:33]([C:29]([CH3:32])([CH3:31])[CH3:30])[C:34]([NH2:24])=[O:35])=[CH:7][N:8]=[C:9]2[CH3:21])=[CH:13][C:14]=1[F:20])#[N:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 62412tert-Butyl isocyanateHCID 226271114-[5-(2-Amino-ethyl)-2-(methyl)-imidazol-1-ylmethyl]-2-fluoro-benzonitrile dihydrochloride

生成物 1

HCID 21706166{2-[3-(4-cyano-3-fluoro-benzyl)-2-methyl-3H-imidazol-4-yl]-ethyl}-tert-butyl Urea

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4-[5-(2-amino-ethyl)-2-methyl-imidazol-1-ylmethyl]-2-fluoro-benzonitrile dihydrochloride (as described in Example 34, Step A) (0.3 g, 0.97 mmol) in DMF (5.0 mL) was added NEt3 (0.41 mL, 2.97 mmol) and t-butyl-isocyanate (0.125 mL, 1.07 mmol). After ½ hr the DMF was removed in vacuo and the residue partitioned between EtOAc and saturated NaHCO3. The organic layer was separated, washed with brine and dried (MgSO4). Filtration and concentration in vacuo gave the title compound as an oil.

後処理

  1. customAfter ½ hr the DMF was removed in vacuo
  2. customthe residue partitioned between EtOAc and saturated NaHCO3
  3. customThe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried (MgSO4)
  6. filtrationFiltration and concentration in vacuo

出典と根拠

ORDレコード
ord-6de85fadb4b34957932e0455cfd2474d
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06284755B1

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート