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Piperazine → HCID 14128502、化合物

HRID 621574
ノート
印刷プレビュー

反応式

HRID 621574 の反応式
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:7]=1[CH2:8][CH2:9][C:10](=[O:16])[NH:11]2.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C([O-])(O)=O.[Na+]>>[N:17]1([CH2:2][CH2:3][CH2:4][O:5][C:6]2[CH:15]=[CH:14][CH:13]=[C:12]3[C:7]=2[CH2:8][CH2:9][C:10](=[O:16])[NH:11]3)[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 4837PiperazineHCID 516892Sodium BicarbonateHCID 12899139HCID 12899139、化合物

生成物 1

HCID 14128502HCID 14128502、化合物収率 49.7%

実験手順

(a)-1 3.0 grams of 5-(3-chloropropoxy)-3,4-dihydrocarbostyril and 10 g of piperazine are mixed with 20 ml of hexamethylphosphoryl triamide and heated at 80°-90° C. for 5 hours. The reaction mixture is distilled under a reduced pressure to remove hexamethylphosphoryl triamide and unreacted piperazine. To the residue thus obtained are added 30 ml of 5%-NaHCO3 aqueous solution, followed by extraction with chloroform. The chloroform layer is washed with water and chloroform is removed by distillation. The residue thus obtained is purified by silica-gel chromatography to obtain 1.8 g of 5-(3-piperazinylpropoxy)-3,4-dihydrocarbostyril having a melting point of 192°-195° C.

後処理

  1. temperatureheated at 80°-90° C. for 5 hours
  2. distillationThe reaction mixture is distilled under a reduced pressure
  3. customto remove hexamethylphosphoryl triamide and unreacted piperazine
  4. customTo the residue thus obtained
  5. extractionfollowed by extraction with chloroform
  6. washThe chloroform layer is washed with water and chloroform
  7. customis removed by distillation
  8. customThe residue thus obtained
  9. customis purified by silica-gel chromatography

出典と根拠

ORDレコード
ord-43e9f53517924ca99085d57bf35da754
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04824840

反応ノート

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