Cesium carbonate → HCID 9823286、化合物

HRID 379071ノート

反応式

HRID 379071 の反応式
C(=O)([O-])[O-].[Cs+].[Cs+].[OH:7][C:8]1[CH:15]=[C:14]([CH2:16][N:17]2[CH:21]=[CH:20][N:19]=[CH:18]2)[CH:13]=[CH:12][C:9]=1[C:10]#[N:11].Br[CH2:23][C:24]1[CH:25]=[CH:26][C:27]([N:30]2[CH:35]=[C:34]([Cl:36])[CH:33]=[CH:32][C:31]2=[O:37])=[N:28][CH:29]=1>CN(C=O)C>[Cl:36][C:34]1[CH:33]=[CH:32][C:31](=[O:37])[N:30]([C:27]2[CH:26]=[CH:25][C:24]([CH2:23][O:7][C:8]3[CH:15]=[C:14]([CH2:16][N:17]4[CH:21]=[CH:20][N:19]=[CH:18]4)[CH:13]=[CH:12][C:9]=3[C:10]#[N:11])=[CH:29][N:28]=2)[CH:35]=1

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 21696991HCID 21696991、化合物HCID 216970282-Hydroxy-4-imidazol-1-ylmethyl-benzonitrile

生成物 1

HCID 9823286HCID 9823286、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Cesium carbonate (0.123 g, 0.376 mmol) was added to a solution of 2-hydroxy-4-imidazol-1-ylmethyl-benzonitrile (as described in Example 4, Step F) (0.050 g, 0.25 mmol) and 5′-bromomethyl-5-chloro-[1,2′]bipyridinyl-2-one (Step H) (0.079 g, 0.263 mmol) in anhydrous DMF (5 mL) and stirred at ambient temperature overnight. The reaction mixture was partitioned between EtOAc and aqueous saturated NaHCO3 solution, the organic layer separated, washed with H2O, brine and dried (MgSO4). Filtration and concentration to dryness gave the title compound after chromatography (silica gel, 1-4% CH3OH/CH2Cl2). FAB MS 418 (M+1).

後処理

  1. customThe reaction mixture was partitioned between EtOAc and aqueous saturated NaHCO3 solution
  2. customthe organic layer separated
  3. washwashed with H2O, brine
  4. dry with materialdried (MgSO4)
  5. filtrationFiltration and concentration to dryness

出典と根拠

ORDレコード
ord-3c7eeeaae4ba4a1e9ca2ae98c658e065
出典データセット
uspto-grants-2001_10
特許番号
US06297239B1

反応ノート

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