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

HRID 569960

반응식

HRID 569960 반응식
[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]

참가 물질

8

반응물 4

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

생성물 1

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

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 702Ethanol용매2회HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-313bd711b4194964864aa7d800bcb0d7
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04734416

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