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Potassium Carbonate → 3-Methyl-2-[4-[6-(4-piperidinopiperidino)nicotinoyl]benzylthio]-4H-pyrido[1,2-a]pyrimidin-4-one trihydrochloride

HRID 1291390
ノート
印刷プレビュー

反応式

HRID 1291390 の反応式
[Cl:1][C:2]1[CH:29]=[CH:28][C:5]([C:6]([C:8]2[CH:27]=[CH:26][C:11]([CH2:12][S: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][N:3]=1.[N:30]1([CH:36]2[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]2)[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[ClH:1].[ClH:1].[ClH:1].[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[S:13][CH2:12][C:11]1[CH:26]=[CH:27][C:8]([C:6](=[O:7])[C:5]2[CH:28]=[CH:29][C:2]([N:39]3[CH2:40][CH2:41][CH:36]([N:30]4[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]4)[CH2:37][CH2:38]3)=[N:3][CH:4]=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 786071,4'-BipiperidineHCID 189190212-[4-(6-Chloronicotinoyl]benzylthio]-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

生成物 1

HCID 189189983-Methyl-2-[4-[6-(4-piperidinopiperidino)nicotinoyl]benzylthio]-4H-pyrido[1,2-a]pyrimidin-4-one trihydrochloride収率 18.6%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A solution of 2-[4-(6-chloronicotinoyl)benzylthio]-3-methyl-4H-pyrido[1,2-a]-pyrimidin-4-one (287 mg), 4-piperidinopiperidine (137 mg) and potassium carbonate (194 mg) in DMF (10 ml) was stirred at 80° C. for 24 hours. This reaction mixture was concentrated and the residue was dissolved in chloroform. The solution was washed with water, dried, and concentrated. The residue was purified by silica gel column chromatography (chloroform-methanol =9:1) and treated with hydrogen chloride/ethyl acetate to provide the title compound as colorless solid (28 mg).

後処理

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in chloroform
  3. washThe solution was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (chloroform-methanol =9:1)
  7. additiontreated with hydrogen chloride/ethyl acetate

出典と根拠

ORDレコード
ord-07e5dac7407b4e19b143ddc6d00b9848
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

読み込み中…

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