Sodium Chloride → HCID 9807043、化合物

HRID 1384340ノート

反応式

HRID 1384340 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([C:18]([C:26]4[CH:27]=[N:28][C:29]([Cl:32])=[CH:30][CH:31]=4)([OH:25])[C:19]4[N:20]([CH3:24])[CH:21]=[N:22][CH:23]=4)[CH:16]=3)[NH:11][C:10](=[O:33])[CH:9]=2)[CH:5]=[CH:6][CH:7]=1.[Na+].[Cl-].C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH2:43][CH:44]1[CH2:46][CH2:45]1>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([C:18]([C:26]4[CH:27]=[N:28][C:29]([Cl:32])=[CH:30][CH:31]=4)([OH:25])[C:19]4[N:20]([CH3:24])[CH:21]=[N:22][CH:23]=4)[CH:16]=3)[N:11]([CH2:43][CH:44]3[CH2:46][CH2:45]3)[C:10](=[O:33])[CH:9]=2)[CH:5]=[CH:6][CH:7]=1

参加物

6

実験手順

To a solution of the title compound of example 1, 4-(3-chloro-phenyl)-6-[(6-chloro-pyridin-3-yl)-hydroxy-(3-methyl-3H-imidazol-4-yl)-methyl]-1H-quinolin-2-one (100 mg, 0.210 mmol) in DMF (2 ml) were added NaCl (8 mg), cesium carbonate (Cs2CO3, 103 mg, 0.315 mmol) and (bromomethyl)cyclopropane (0.041 ml, 0.420 mmol). The reaction mixture was stirred at ambient temperature for 15 hours. Additional 0.041 ml) of (bromomethyl)cyclopropane and 100 mg of Cs2CO were added. The reaction mixture was heated at 60° C. for 1 hour after which time it was partitioned between CHCl3 and water. The organic layer was washed with brine, dried over MgSO4 and concentrated under vacuum to give the crude product. It was chromatographed on silica gel with MeOH—CHCl3—NH4OH (3:97:0) as eluents to afford the title compound as a white solid (25 mg, 22% yield).

出典と根拠

ORDレコード
ord-cd19585bce8944aba01bc0d1f7d80266
出典データセット
uspto-grants-2001_07
特許番号
US06258824B1

反応ノート

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