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1-Bromo-3-chloropropane → HCID 10658563, 화합물

HRID 2256981
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HRID 2256981 반응식
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][C:7](=[O:13])[NH:8]2.[H-].[Na+].[Na].Br[CH2:18][CH2:19][CH2:20][Cl:21]>CN(C)C=O>[Cl:21][CH2:20][CH2:19][CH2:18][N:8]1[C:9]2[C:4](=[C:3]([O:2][CH3:1])[CH:12]=[CH:11][CH:10]=2)[CH2:5][CH2:6][C:7]1=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 80061-Bromo-3-chloropropaneHCID 24758Sodium hydrideHCID 5360545SodiumHCID 129471185-Methoxy-3,4-dihydroquinolin-2(1H)-one2회

생성물 1

HCID 10658563HCID 10658563, 화합물수율 77.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a solution of 5-methoxy-3,4-dihydrocarbostyril (53.1 g, 0.3 mole) in 200 ml of dimethylformamide (DMF) was added portionwise 60% sodium hydride in oil (19.2.g, 0.4 mole) at room temperature, and the mixture was stirred for 30 minutes. To the thus-obtained solution of the sodium salt of 5-methoxy-3,4-dihydrocarbostyril in DMF was added 1-bromo-3-chloropropane (94 ml, 0.6 mole). The mixture was stirred at 80°-90° C. for 8 hours. The DMF was distilled off under reduced pressure, and the residue was extracted with chloroform. The extract was washed with water and dried (anhydrous magnesium sulfate), the chloroform was distilled off under reduced pressure, and the residue was recrystallized from ethanol to give 59 g of 1-(3-chloropropyl)-5-methoxy-3,4-dihydrocarbostyril as colorless needles.

후처리

  1. stirringThe mixture was stirred at 80°-90° C. for 8 hours
  2. distillationThe DMF was distilled off under reduced pressure
  3. extractionthe residue was extracted with chloroform
  4. washThe extract was washed with water
  5. dry with materialdried (anhydrous magnesium sulfate)
  6. distillationthe chloroform was distilled off under reduced pressure
  7. customthe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-9cad462ba2574b48bcb9cab992589fd0
출처 데이터셋
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05656633

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