Hydrochloric Acid → 7-{3-[4-(3,4,5-Trimethoxyphenyl)-piperazinyl]propoxy}-3,4-dihydrocarbostyril dihydrochloride

HRID 569960

反応式

HRID 569960 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:15]=[C:14]2[C:9]([CH2:10][CH2:11][C:12](=[O:16])[NH:13]2)=[CH:8][CH:7]=1.[CH3:17][O:18][C:19]1[CH:20]=[C:21]([N:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)[CH:22]=[C:23]([O:27][CH3:28])[C:24]=1[O:25][CH3:26].C(=O)([O-])O.[Na+].[ClH:40]>CS(C)=O.C(O)C.N1C=CC=CC=1>[ClH:1].[ClH:40].[CH3:28][O:27][C:23]1[CH:22]=[C:21]([N:29]2[CH2:34][CH2:33][N:32]([CH2:2][CH2:3][CH2:4][O:5][C:6]3[CH:15]=[C:14]4[C:9]([CH2:10][CH2:11][C:12](=[O:16])[NH:13]4)=[CH:8][CH:7]=3)[CH2:31][CH2:30]2)[CH:20]=[C:19]([O:18][CH3:17])[C:24]=1[O:25][CH3:26]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 38387651-(3,4,5-Trimethoxyphenyl)piperazineHCID 130535297-(3-Chloropropoxy)-3,4-dihydroquinolin-2(1H)-one

生成物 1

HCID 128995267-{3-[4-(3,4,5-Trimethoxyphenyl)-piperazinyl]propoxy}-3,4-dihydrocarbostyril dihydrochloride収率 61%

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 702Ethanol溶媒2 回HCID 1049Pyridine溶媒

実験手順

12.4 Grams of 7-(3-chloropropoxy)-3,4-dihydrocarbostyril, 1 g of pyridine and 2.6 g of 4-(3,4,5-trimethoxyphenyl)piperazine are mixed in 20 ml of dimethylsulfoxide, then stirred at 80°-90° C. for 5 hours. The reaction mixture is poured into 80 ml of 2% aqueous solution of sodium hydrogencarbonate and the organic layer is extracted with chloroform. The chloroform layer is washed with water, dried and chloroform is removed by distillation. The residue thus obtained is dissolved in 30 ml of ethanol and dried hydrogen chloride gas is blown into the ethanol solution. The crystals thus precipitated are collected by filtration and recrystallized from methanol-ethanol to obtain 3.2 g (yield: 61%) of 7-{3-[4-(3,4,5-trimethoxyphenyl)piperazinyl]propoxy}-3,4-dihydrocarbostyril dihydrochloride in the form of colorless needle-like crystals with a melting point of 225°-227° C.

後処理

  1. extractionthe organic layer is extracted with chloroform
  2. washThe chloroform layer is washed with water
  3. customdried
  4. customchloroform is removed by distillation
  5. customThe residue thus obtained
  6. customThe crystals thus precipitated
  7. filtrationare collected by filtration
  8. customrecrystallized from methanol-ethanol

出典と根拠

ORDレコード
ord-313bd711b4194964864aa7d800bcb0d7
出典データセット
uspto-grants-1988_03
特許番号
US04734416

関連ノート

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