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Potassium Iodide → 3-[2-[4-[(2-fluorophenyl)(2-phenylhydrazono)methyl]-1-piperazinyl]ethyl]-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

HRID 2051015
ノート
印刷プレビュー

反応式

HRID 2051015 の反応式
Cl[CH2:2][CH2:3][C:4]1[C:9](=[O:10])[N:8]2[CH:11]=[CH:12][CH:13]=[CH:14][C:7]2=[N:6][C:5]=1[CH3:15].[F:16][C:17]1[CH:30]=[CH:29][CH:28]=[CH:27][C:18]=1[C:19]([N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1)=O.[C:31]1([NH:37][NH2:38])[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>CC(C)CC(=O)C>[F:16][C:17]1[CH:30]=[CH:29][CH:28]=[CH:27][C:18]=1[C:19](=[N:38][NH:37][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[N:21]1[CH2:26][CH2:25][N:24]([CH2:2][CH2:3][C:4]2[C:9](=[O:10])[N:8]3[CH:11]=[CH:12][CH:13]=[CH:14][C:7]3=[N:6][C:5]=2[CH3:15])[CH2:23][CH2:22]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 4875Potassium IodideHCID 7516PhenylhydrazineHCID 10340Sodium CarbonateHCID 544862(2-Fluoro-phenyl)-piperazin-1-yl-methanoneHCID 8178663-(2-Chloroethyl)-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

生成物 1

HCID 566196993-[2-[4-[(2-fluorophenyl)(2-phenylhydrazono)methyl]-1-piperazinyl]ethyl]-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

A mixture of 4.5 parts of 3-(2-chloroethyl)-2-methyl-4H-pyrido-[1,2-a]pyrimidin-4-one, 6 parts of 1-(2-fluorobenzoyl)piperazine, 2-phenylhydrazine, 5.04 parts of sodium carbonate, 0.1 parts of potassium iodide and 120 parts of 4-methyl-2-pentanone was stirred overnight at reflux temperature. The inorganic salts were filtered off and the filtrate was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2-propanol. The product was filtered off and dried, yielding 2.5 parts (25.8) of 3-[2-[4-[(2-fluorophenyl)(2-phenylhydrazono)methyl]-1-piperazinyl]ethyl]-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one; mp. 180° C. (int. 10).

後処理

  1. temperatureat reflux temperature
  2. filtrationThe inorganic salts were filtered off
  3. customthe filtrate was evaporated
  4. customThe residue was purified by column chromatography over silica gel using
  5. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
  6. customThe pure fractions were collected
  7. customthe eluent was evaporated
  8. customThe residue was crystallized from 2-propanol
  9. filtrationThe product was filtered off
  10. customdried

出典と根拠

ORDレコード
ord-79145bf9ba0c47d08a5d7cfbfc7b49b9
出典データセット
uspto-grants-1991_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05015740

反応ノート

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