Hydrochloric Acid → 3,4-Dihydrocarbostyril hydrochloride

HRID 1263117노트

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HRID 1263117 반응식
O=C([C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12](=[O:17])[CH2:11][CH2:10]2)CCC[Cl:6].[I-].[Na+].C1OC2C=CC(N3CCNCC3)=CC=2O1.C1CCN2C(=NCCC2)CC1.C(=O)([O-])O.[Na+].Cl>CS(C)=O.CO>[ClH:6].[NH:13]1[C:14]2[C:9](=[CH:8][CH:7]=[CH:16][CH:15]=2)[CH2:10][CH2:11][C:12]1=[O:17]

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 5238Sodium IodideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 516892Sodium BicarbonateHCID 47420031-(1,3-Benzodioxol-5-yl)piperazineHCID 128335166-(4-Chlorobutyryl)-3,4-dihydrocarbostyril

생성물 1

HCID 189587973,4-Dihydrocarbostyril hydrochloride

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 887Methanol용매

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온도
50 °C

실험 절차

2.7 Grams of 6-(1-oxo-4-chlorobutyl)-3,4-dihydrocarbostyril and 1.5 g of sodium iodide were mixed in 30 ml of dimethyl sulfoxide and the mixture was stirred at 50° C. for 2 hours. Then to the reaction mixture were added 2.0 g of 4-(3,4-methylenedioxyphenyl)-piperazine and 3 g of DBU and the reaction mixture was stirred at 70°-80° C. for 5 hours. After the reaction was completed, the reaction mixture was poured into 10 ml of 2%-sodium hydrogencarbonate and the organic layer was extracted with chloroform. The chloroform layer was washed with water, dried and chloroform was removed by distillation. To the residue thus obtained were added 50 ml of methanol and 5 ml of concentrated hydrochloric acid and the mixture was concentrated under a reduced pressure to dryness. The residue thus obtained was crystallized by adding ethanol-acetone to obtain crude crystals, and the crude crystals were recrystallized from ethanol-water. 2.1 Grams of 6-{1-oxo-4-(3,4-methylenedioxy-phenyl)-1-piperazinyl]butyl}-3,4-dihydrocarbostyril monohydrochloride in colorless powdery crystals were obtained.

후처리

  1. stirringthe reaction mixture was stirred at 70°-80° C. for 5 hours
  2. extractionthe organic layer was extracted with chloroform
  3. washThe chloroform layer was washed with water
  4. customdried
  5. customchloroform was removed by distillation
  6. customTo the residue thus obtained
  7. concentrationthe mixture was concentrated under a reduced pressure to dryness
  8. customThe residue thus obtained
  9. customwas crystallized
  10. additionby adding ethanol-acetone
  11. customto obtain crude crystals
  12. customthe crude crystals were recrystallized from ethanol-water

출처 및 근거

ORD 기록
ord-44af66fdb88846b485de50c8115d62fd
출처 데이터셋
uspto-grants-1984_06
특허 번호
US04455422

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