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Hydrochloric Acid → 6-(4-Chloro-1-butenyl)-3,4-dihydrocarbostyril

HRID 1285415
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HRID 1285415 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([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)=O.[BH4-].[Na+].Cl>CO>[Cl:1][CH2:2][CH2:3][CH:4]=[CH:5][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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 128335166-(4-Chlorobutyryl)-3,4-dihydrocarbostyril

생성물 1

HCID 544375796-(4-Chloro-1-butenyl)-3,4-dihydrocarbostyril

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4.0 Grams of 6-(4-chloro-1-oxobutyl)-3,4-dihydrocarbostyril was disposed in 200 ml of methanol, and the suspension was stirred at a room temperature. Then 2.0 g of sodium borohydride was added to the suspension gradually and the reaction was continued for 1 hour. Next, 3 ml of concentrated hydrochloric acid was added to the reaction mixture and the mixture was concentrated under a reduce pressure with heat-refluxing condition to obtain a residue. The residue was extracted with chloroform and the chloroform layer was washed with water and dried. Then colorform was removed by distillation under a reduced pressure to obtain a residue, and the residue was recrystallized from ethanol to obtain 2.4 g of 6-(4-chloro-1-butenyl)-3,4-dihydrocarbostyril in yellow needle-like crystals. Melting point: 153°-155° C.

후처리

  1. concentrationthe mixture was concentrated under a reduce pressure
  2. temperaturewith heat-refluxing condition
  3. customto obtain a residue
  4. extractionThe residue was extracted with chloroform
  5. washthe chloroform layer was washed with water
  6. customdried
  7. customThen colorform was removed by distillation under a reduced pressure
  8. customto obtain a residue
  9. customthe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-08a536a305654fe09360f528d707e7f8
출처 데이터셋
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04567187

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