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Potassium Carbonate → (R)-5-Dipropylamino-1-methoxy-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one

HRID 901811
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HRID 901811 반응식
[CH2:1]([NH:4][C@@H:5]1[CH2:14][C:13]2[C:8]3=[C:9]([N:15]([O:18][CH3:19])[C:16](=[O:17])[N:7]3[CH2:6]1)[CH:10]=[CH:11][CH:12]=2)[CH2:2][CH3:3].I[CH2:21][CH2:22][CH3:23].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:1]([N:4]([CH2:21][CH2:22][CH3:23])[C@@H:5]1[CH2:14][C:13]2[C:8]3=[C:9]([N:15]([O:18][CH3:19])[C:16](=[O:17])[N:7]3[CH2:6]1)[CH:10]=[CH:11][CH:12]=2)[CH2:2][CH3:3]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 336431-Iodopropane2회HCID 10286043HCID 10286043, 화합물

생성물 1

HCID 9817922(R)-5-Dipropylamino-1-methoxy-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one수율 90%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Following the procedure of Example 3, a mixture of (R)-5-Propylamino-1-methoxy-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one (8b, 0.93 g,3.56 mmol), 1-iodopropane (3.05 g, 17.9 mmol), and potassium carbonate (1.97 g, 14.3 mmol) in acetonitrile (25 ml) was heated at reflux under nitrogen for 17 hours. 1-Iodopropane (3.05 g, 17.9 mmol) was again added, and the mixture was refluxed for an additional 5 hours. The solvent was removed under vacuum, and the mixture was diluted with water and extracted twice with diethylether. The organic extract was washed with brine and dried (MgSO4). The solvent was removed under vacuum to leave an amber oil. Purification by flash chromatography (230-400 mesh silica gel; 10-25% ethyl acetate in hexane) gave the title compound (9b) as an amber oil (0.87 g, 90% yield).

후처리

  1. temperaturewas heated
  2. temperatureat reflux under nitrogen for 17 hours
  3. temperaturethe mixture was refluxed for an additional 5 hours
  4. customThe solvent was removed under vacuum
  5. additionthe mixture was diluted with water
  6. extractionextracted twice with diethylether
  7. extractionThe organic extract
  8. washwas washed with brine
  9. dry with materialdried (MgSO4)
  10. customThe solvent was removed under vacuum
  11. customto leave an amber oil
  12. customPurification by flash chromatography (230-400 mesh silica gel; 10-25% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-19028279e9ee460fba15321cb5671849
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE040278E1

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