1-(m-Tolyl)piperazine → HCID 12414812、化合物

HRID 1657409ノート

反応式

HRID 1657409 の反応式
Cl[CH2:2][CH2:3][C:4]1[C:9](=[O:10])[N:8]2[CH:11]=[C:12]([CH3:15])[CH:13]=[CH:14][C:7]2=[N:6][C:5]=1[CH3:16].[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>[C:17]1([CH3:29])[CH:22]=[CH:21][CH:20]=[C:19]([N:23]2[CH2:24][CH2:25][N:26]([CH2:2][CH2:3][C:4]3[C:9](=[O:10])[N:8]4[CH:11]=[C:12]([CH3:15])[CH:13]=[CH:14][C:7]4=[N:6][C:5]=3[CH3:16])[CH2:27][CH2:28]2)[CH:18]=1

参加物

4

反応物 2

HCID 831111-(m-Tolyl)piperazineHCID 124149363-(2-Chloroethyl)-2,7-dimethyl-4H-pyrido[1,2-a]pyrimidin-4-one

生成物 1

HCID 12414812HCID 12414812、化合物収率 57.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 2.2 g of 3-(2-chloroethyl)-2,7-dimethyl-4H-pyrido[1,2-a]pyrimidin-4-one, 5 g of 1-(m-tolyl)piperazine and 25 ml of toluene was refluxed for 30 hours. After completion of the reaction, the reaction mixture was filtered while hot and the filtrate was concentrated under reduced pressure. The residue was purified by means of column chromatography using alumina and recrystallized from a mixture of ethanol and isopropyl ether to give 2 g of the desired compound as pale yellow prisms, m.p. 115 - 116°C.

後処理

  1. temperaturewas refluxed for 30 hours
  2. customAfter completion of the reaction
  3. filtrationthe reaction mixture was filtered while hot and the filtrate
  4. concentrationwas concentrated under reduced pressure
  5. customThe residue was purified by means of column chromatography
  6. customrecrystallized from a mixture of ethanol and isopropyl ether

出典と根拠

ORDレコード
ord-3659aeb59ddc440aba773ac9789dd5dc
出典データセット
uspto-grants-1976_06
特許番号
US03960863

反応ノート

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