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

HRID 1291388
ノート
印刷プレビュー

反応式

HRID 1291388 の反応式
[OH:1][C:2]1[CH:29]=[CH:28][C:5]([C:6]([C:8]2[CH:27]=[CH:26][C:11]([CH2:12][O:13][C:14]3[N:15]=[C:16]4[CH:25]=[CH:24][CH:23]=[CH:22][N:17]4[C:18](=[O:21])[C:19]=3[CH3:20])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.Cl.[N:31]1[CH:36]=[CH:35][C:34]([CH2:37][Cl:38])=[CH:33][CH:32]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[ClH:38].[CH3:20][C:19]1[C:18](=[O:21])[N:17]2[CH:22]=[CH:23][CH:24]=[CH:25][C:16]2=[N:15][C:14]=1[O:13][CH2:12][C:11]1[CH:26]=[CH:27][C:8]([C:6](=[O:7])[C:5]2[CH:4]=[CH:3][C:2]([O:1][CH2:37][C:34]3[CH:35]=[CH:36][N:31]=[CH:32][CH:33]=3)=[CH:29][CH:28]=2)=[CH:9][CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 745704-(Chloromethyl)pyridinium chlorideHCID 189188752-[4-(4-hydroxybenzoyl)benzyloxy]-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

生成物 1

HCID 189189243-Methyl-2-[4-[4-(4-picolyloxy)benzoyl]benzyloxy]-4H-pyrido[1,2-a]pyrimidin-4-one hydrochloride収率 68.1%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A solution of 2-[4-(4-hydroxybenzoyl)benzyloxy]-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (96 mg), 4-picolyl chloride hydrochloride (89 mg) and potassium carbonate (178 mg) in DMF (7 ml) was stirred at room temperature for 13 hours. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate, washed with water, dried, and concentrated. The residue was purified by silica gel column chromatography (dichloromethane: methanol =20:1) and treated with hydrogen chloride/ethyl acetate to provide the title compound as colorless solid (87 mg).

後処理

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (dichloromethane: methanol =20:1)
  7. additiontreated with hydrogen chloride/ethyl acetate

出典と根拠

ORDレコード
ord-8e2b41665e174c589f379865b90ad776
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05753664

反応ノート

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