Potassium Carbonate → 2-[4-(4-hydroxybenzoyl)benzyloxy]-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

HRID 1291393ノート

反応式

HRID 1291393 の反応式
[OH: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].[Si]([O:21][C:22]1[CH:37]=[CH:36][C:25]([C:26]([C:28]2[CH:35]=[CH:34][C:31]([CH2:32]Br)=[CH:30][CH:29]=2)=[O:27])=[CH:24][CH:23]=1)(C(C)(C)C)(C)C.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[O:1][CH2:32][C:31]1[CH:30]=[CH:29][C:28]([C:26](=[O:27])[C:25]2[CH:36]=[CH:37][C:22]([OH:21])=[CH:23][CH:24]=2)=[CH:35][CH:34]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 18918912HCID 18918912、化合物HCID 135448456HCID 135448456、化合物

生成物 1

HCID 189188752-[4-(4-hydroxybenzoyl)benzyloxy]-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one収率 4.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2-hydroxy-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (3.158 g), 4-(4-t-butyldimethylsilyloxybenzoyl)benzyl bromide (12.24 g) and potassium carbonate (5.07 g) in DMF (50 ml) was stirred at room temperature for 24 hours. This reaction mixture was concentrated and the residue was purified by silica gel column chromatography (dichloromethane: ethyl acetate =1:2) and recrystallized from chloroform-methanol-ethyl acetate to provide the title compound as colorless solid (325 mg).

後処理

  1. concentrationThis reaction mixture was concentrated
  2. customthe residue was purified by silica gel column chromatography (dichloromethane: ethyl acetate =1:2)
  3. customrecrystallized from chloroform-methanol-ethyl acetate

出典と根拠

ORDレコード
ord-2e836f995f4b49089e9108168dc40fae
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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