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Diethyl Ether → 6-(1-Oxo-2-morpholinoethyl)-3,4-dihydrocarbostyril monohydrochloride

HRID 1462545
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HRID 1462545 반응식
[O:1]=[C:2]([C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10](=[O:15])[CH2:9][CH2:8]2)[CH2:3][Cl:4].[NH:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1.CCOCC>O1CCOCC1>[ClH:4].[O:1]=[C:2]([C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10](=[O:15])[CH2:9][CH2:8]2)[CH2:3][N:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1
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참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 8083MorpholineHCID 49617906-(2-Chloroacetyl)-1,2,3,4-tetrahydroquinolin-2-one

생성물 1

HCID 202294546-(1-Oxo-2-morpholinoethyl)-3,4-dihydrocarbostyril monohydrochloride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

5.0 Grams of 6-(1-oxo-2-chloroethyl)-3,4-dihydrocarbostyril and 6.0 g of morpholine were dispersed in 120 ml of dioxane and stirred at 60°-70° C. for 12 hours. The reaction mixture was concentrated under a reduced pressure. The residue thus obtained was stirred with ether and the insoluble matter was collected by filtration and washed with water. Then the insoluble matter was dissolved in 80 ml of methanol and 10 ml of concentrated hydrochloric acid by heating and the solution was concentrated under a reduced pressure to dryness. The residue thus obtained was recrystallized from methanol-ether twice and obtained 5.9 g of 6-(1-oxo-2-morpholinoethyl)-3,4-dihydrocarbostyril monohydrochloride in colorless powdery product.

후처리

  1. concentrationThe reaction mixture was concentrated under a reduced pressure
  2. customThe residue thus obtained
  3. filtrationthe insoluble matter was collected by filtration
  4. washwashed with water
  5. dissolutionThen the insoluble matter was dissolved in 80 ml of methanol
  6. temperature10 ml of concentrated hydrochloric acid by heating
  7. concentrationthe solution was concentrated under a reduced pressure to dryness
  8. customThe residue thus obtained
  9. customwas recrystallized from methanol-ether twice

출처 및 근거

ORD 기록
ord-6fc07453a9654d5fb11cec197b01f721
출처 데이터셋
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04460593

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