Potassium Carbonate → HCID 69192521, 화합물

HRID 1187399노트

반응식

HRID 1187399 반응식
C(=O)([O-])[O-].[K+].[K+].C([O:10][CH2:11][CH2:12][CH2:13][N:14]1[C:26]2[C:25]3[N:24]=[CH:23][CH:22]=[CH:21][C:20]=3[N:19]=[CH:18][C:17]=2[N:16]=[CH:15]1)(=O)C>CO>[N:14]1([CH2:13][CH2:12][CH2:11][OH:10])[C:26]2[C:25]3[N:24]=[CH:23][CH:22]=[CH:21][C:20]=3[N:19]=[CH:18][C:17]=2[N:16]=[CH:15]1

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 69192155HCID 69192155, 화합물

생성물 1

HCID 69192521HCID 69192521, 화합물수율 16.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Solid potassium carbonate (2.68 g, 19.4 mmol) was added to a solution of 3-(1H-imidazo[4,5-c][1,5]naphthyridin-1-yl)propyl acetate (3.50 g, 12.9 mmol) in methanol (65 mL) at room temperature. The mixture was stirred for 3 hours, then the solvent was removed under reduced pressure. The residue was partitioned between dichloromethane (150 mL) and water (75 mL). The organic layer was washed with brine (75 mL), dried over magnesium sulfate, filtered, and concentrated under reduced pressure to yield a brown semi-solid that was triturated with dichloromethane and isolated by filtration to afford 0.48 g of 3-(1H-imidazo[4,5-c][1,5]naphthyridin-1-yl)propan-1-ol. The filtrate was concentrated under reduced pressure, and the residue was purified by chromatography on a HORIZON HPFC system (silica gel, gradient elution with 0-50% CMA in chloroform) to provide an additional 0.67 g of 3-(1H-imidazo[4,5-c][1,5]naphthyridin-1-yl)propan-1-ol.

후처리

  1. customthe solvent was removed under reduced pressure
  2. customThe residue was partitioned between dichloromethane (150 mL) and water (75 mL)
  3. washThe organic layer was washed with brine (75 mL)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customto yield a brown semi-solid that
  8. customwas triturated with dichloromethane
  9. customisolated by filtration

출처 및 근거

ORD 기록
ord-e883643177bb4dc8a7c3a9da9ceb8724
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08673932B2

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