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Potassium Carbonate → ethyl 2-(7-(2,5-dimethyl-1H-pyrrol-1-yl)-2-oxo-3,4-dihydroquinolin-1(2H)-yl)propanoate

HRID 519077
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HRID 519077 반응식
[CH3:1][C:2]1[N:3]([C:8]2[CH:17]=[C:16]3[C:11]([CH2:12][CH2:13][C:14](=[O:18])[NH:15]3)=[CH:10][CH:9]=2)[C:4]([CH3:7])=[CH:5][CH:6]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH:26]([CH3:32])[C:27]([O:29][CH2:30][CH3:31])=[O:28]>C(#N)C>[CH3:1][C:2]1[N:3]([C:8]2[CH:17]=[C:16]3[C:11]([CH2:12][CH2:13][C:14](=[O:18])[N:15]3[CH:26]([CH3:32])[C:27]([O:29][CH2:30][CH3:31])=[O:28])=[CH:10][CH:9]=2)[C:4]([CH3:7])=[CH:5][CH:6]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 79040Ethyl 2-bromopropionateHCID 867274437-(2,5-dimethyl-pyrrol-1-yl)-3,4-dihydro-1H-quinolin-2-one

생성물 1

HCID 86727444ethyl 2-(7-(2,5-dimethyl-1H-pyrrol-1-yl)-2-oxo-3,4-dihydroquinolin-1(2H)-yl)propanoate수율 81%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 7-(2,5-dimethyl-1H-pyrrol-1-yl)-3,4-dihydroquinolin-2(1H)-one (1.4 g, 5.8 mmol) and potassium carbonate (2.4 g, 17.5 mmol) in ACN (40 mL) was stirred for 30 min then ethyl 2-bromopropanoate (2.1 g, 11.6 mmol) was added and the mixture was heated to reflux overnight. The reaction mixture was cooled to ambient temperature and the solvent was removed in vacuo. EtOAc (50 mL) and water (30 mL) was added to the residue and the organic layer was separated, dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by column chromatography on silica gel (eluting with 0-30% EtOAc in petroleum ether) to give ethyl 2-(7-(2,5-dimethyl-1H-pyrrol-1-yl)-2-oxo-3,4-dihydroquinolin-1(2H)-yl)propanoate (1.6 g, 81%). 1H NMR (CDCl3, 400 MHz): δ 7.26 (d, J=7.2 Hz, 1H), 6.87 (d, J=7.6 Hz, 1H), 6.71 (s, 1H), 5.91 (s, 2H), 4.98 (q, J=6.8 Hz, 1H), 4.17 (q, J=7.2 Hz, 2H), 2.96 (m, 2H), 2.72 (m, 2H), 2.05 (s, 6H), 1.61 (d, J=7.2 Hz, 3H), 1.19 (t, J=7.2 Hz, 3H).

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux overnight
  3. customthe solvent was removed in vacuo
  4. additionEtOAc (50 mL) and water (30 mL) was added to the residue
  5. customthe organic layer was separated
  6. dry with materialdried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by column chromatography on silica gel (eluting with 0-30% EtOAc in petroleum ether)

출처 및 근거

ORD 기록
ord-b1381cf3d9844362832465aa3be8a088
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115151B2

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