Potassium Carbonate → 3-Methyl-2-[4-[4-(4-phenylpiperazinylmethyl)-benzoyl]benzylthio]-4H-pyrido[1,2-a]pyrimidin-4-one

HRID 1291391ノート

反応式

HRID 1291391 の反応式
[SH:1][C:2]1[N:3]=[C:4]2[CH:13]=[CH:12][CH:11]=[CH:10][N:5]2[C:6](=[O:9])[C:7]=1[CH3:8].Br[CH2:15][C:16]1[CH:31]=[CH:30][C:19]([C:20]([C:22]2[CH:27]=[CH:26][C:25]([CH2:28]Br)=[CH:24][CH:23]=2)=[O:21])=[CH:18][CH:17]=1.Cl.[C:33]1([N:39]2[CH2:44][CH2:43][NH:42][CH2:41][CH2:40]2)[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:8][C:7]1[C:6](=[O:9])[N:5]2[CH:10]=[CH:11][CH:12]=[CH:13][C:4]2=[N:3][C:2]=1[S:1][CH2:15][C:16]1[CH:31]=[CH:30][C:19]([C:20](=[O:21])[C:22]2[CH:27]=[CH:26][C:25]([CH2:28][N:42]3[CH2:43][CH2:44][N:39]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)[CH2:40][CH2:41]3)=[CH:24][CH:23]=2)=[CH:18][CH:17]=1

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 751641-Phenylpiperazinium chlorideHCID 23039244,4'-Bis(bromomethyl)benzophenoneHCID 189188982-mercapto-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

生成物 1

HCID 189188383-Methyl-2-[4-[4-(4-phenylpiperazinylmethyl)-benzoyl]benzylthio]-4H-pyrido[1,2-a]pyrimidin-4-one収率 16.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2-mercapto-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (298 mg), 4,4'-bis(bromomethyl)benzophenone (934 mg), phenylpiperazine hydrochloride (402 mg) and potassium carbonate (850 mg) in DMF (30 ml) was stirred at room temperature for 10 hours. This reaction mixture was concentrated and the residue was dissolved in chloroform, washed with water, dried, and concentrated. The residue was purified by silica gel column chromatography (hexane: ethyl acetate =1:1) to provide the title compound as colorless solid (146 mg).

後処理

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in chloroform
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (hexane: ethyl acetate =1:1)

出典と根拠

ORDレコード
ord-53b480fb6d644aada34800c6e783f814
出典データセット
uspto-grants-1998_05
特許番号
US05753664

反応ノート

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