1-(m-Tolyl)piperazine → 2-Methyl-3-[2-(4-m-tolyl-1-piperazinyl)ethyl]-7-chloro-4H-pyrido[1,2-a]pyrimidin-4-one

HRID 1657407

反応式

HRID 1657407 の反応式
[CH3:1][C:2]1[N:3]=[C:4]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][N:5]2[C:6](=[O:11])[C:7]=1[CH2:8][CH2:9]Cl.[C:17]1([CH3:29])[CH:22]=[CH:21][CH:20]=[C:19]([N:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)[CH:18]=1>C1(C)C=CC=CC=1>[CH3:1][C:2]1[N:3]=[C:4]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][N:5]2[C:6](=[O:11])[C:7]=1[CH2:8][CH2:9][N:26]1[CH2:27][CH2:28][N:23]([C:19]2[CH:18]=[C:17]([CH3:29])[CH:22]=[CH:21][CH:20]=2)[CH2:24][CH2:25]1

参加物

4

反応物 2

HCID 831111-(m-Tolyl)piperazineHCID 124149402-methyl-3-(2-chloroethyl)-7-chloro-4H-pyrido[1,2-a]pyrimidin-4-one

生成物 1

HCID 124148532-Methyl-3-[2-(4-m-tolyl-1-piperazinyl)ethyl]-7-chloro-4H-pyrido[1,2-a]pyrimidin-4-one収率 39.9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 1.3 g of 2-methyl-3-(2-chloroethyl)-7-chloro-4H-pyrido[1,2-a]pyrimidin-4-one, 2.1 g of 1-(m-tolyl)piperazine and 20 ml of toluene was refluxed for 30 hours. After completion of the reaction, the reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The obtained residue was purified by means of column chromatography using alumina and recrystallized from a mixture of ethanol and n-hexane to give 0.8 g of the desired compound as pale yellow scales, m.p. 119° - 120°C.

後処理

  1. temperaturewas refluxed for 30 hours
  2. customAfter completion of the reaction
  3. filtrationthe reaction mixture was filtered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe obtained residue was purified by means of column chromatography
  6. customrecrystallized from a mixture of ethanol and n-hexane

出典と根拠

ORDレコード
ord-b2a14c58a0274586a01eddf82c134411
出典データセット
uspto-grants-1976_06
特許番号
US03960863

関連ノート

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