1-(2-Methoxyphenyl)piperazine → HCID 15136107、化合物

HRID 1651042ノート

反応式

HRID 1651042 の反応式
[CH2:1]([O:3][C:4]([C:6]1[C:11](=[O:12])[N:10]2[CH:13]=[CH:14][CH:15]=[C:16]([SH:17])[C:9]2=[N:8][CH:7]=1)=[O:5])[CH3:2].Cl[C:19](OC(Cl)(Cl)Cl)=[O:20].[CH3:26][O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[N:34]1[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]1>C(Cl)Cl>[CH2:1]([O:3][C:4]([C:6]1[C:11](=[O:12])[N:10]2[CH:13]=[CH:14][CH:15]=[C:16]([S:17][C:19]([N:37]3[CH2:38][CH2:39][N:34]([C:29]4[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=4[O:27][CH3:26])[CH2:35][CH2:36]3)=[O:20])[C:9]2=[N:8][CH:7]=1)=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 13461-(2-Methoxyphenyl)piperazineHCID 10426DiphosgeneHCID 143064713-ethoxycarbonyl-9-mercapto-4H-pyrido[1,2-a]pyrimidin-4-one

生成物 1

HCID 15136107HCID 15136107、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 1.0 g (4 mmol) of 3-ethoxycarbonyl-9-mercapto-4-oxo-4H-pyrido[1,2-a]pyrimidine (II-1) in 40 ml of dry methylene chloride is added 0.24 ml (2 mmol) of trichloromethyl chloroformate, and the resultant mixture is stirred for 10 min. and concentrated at room temperature under atmospheric pressure. To the residue are added 60 ml of dry methylene chloride and 0.77 ml (44 mmol) of 4-(2-methoxyphenyl)piperazine under ice-cooling, and the reaction mixture is stirred for 1 hour at room temperature. The reaction mixture is washed with N--HCl, saturated aqueous NaHCO3 and water in order, and the organic layer is dried and concentrated under reduced pressure. The oily residue in 1.94 g is chromatographed on a column of silica gel eluting with ethyl acetate to give 45 mg of Ia-2 (m.p. 154°-156° C. recrystallized from chloroform-n-hexane) and 516 mg of IV-2 (m.p. 151°-153° C. recrystallized from ethyl acetate).

後処理

  1. concentrationconcentrated at room temperature under atmospheric pressure
  2. temperaturecooling
  3. washThe reaction mixture is washed with N
  4. dry with materialHCl, saturated aqueous NaHCO3 and water in order, and the organic layer is dried
  5. concentrationconcentrated under reduced pressure
  6. customThe oily residue in 1.94 g is chromatographed on a column of silica gel eluting with ethyl acetate
  7. customto give
  8. custom45 mg of Ia-2 (m.p. 154°-156° C. recrystallized from chloroform-n-hexane) and 516 mg of IV-2 (m.p. 151°-153° C. recrystallized from ethyl acetate)

出典と根拠

ORDレコード
ord-a0e0a7cd77664a41a400a8721b477e46
出典データセット
uspto-grants-1990_05
特許番号
US04927829

反応ノート

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