Cesium carbonate → HCID 9823286, 화합물

HRID 379071노트

반응식

HRID 379071 반응식
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

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 21696991HCID 21696991, 화합물HCID 216970282-Hydroxy-4-imidazol-1-ylmethyl-benzonitrile

생성물 1

HCID 9823286HCID 9823286, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3c7eeeaae4ba4a1e9ca2ae98c658e065
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06297239B1

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