Sodium carbonate bicarbonate → 3-(7-Methoxy-4-methyl-2-oxoquinolin-1(2H)-yl)propanal

HRID 1847095노트

반응식

HRID 1847095 반응식
[O:1]1CCO[CH:2]1[CH2:6][CH2:7][N:8]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([O:18][CH3:19])[CH:16]=2)[C:11]([CH3:20])=[CH:10][C:9]1=[O:21].C(=O)([O-])[O-].[Na+].[Na+].C(=O)([O-])O>Cl>[CH3:19][O:18][C:15]1[CH:16]=[C:17]2[C:12]([C:11]([CH3:20])=[CH:10][C:9](=[O:21])[N:8]2[CH2:7][CH2:6][CH:2]=[O:1])=[CH:13][CH:14]=1

참가 물질

4

반응물 2

HCID 86624777Sodium carbonate bicarbonateHCID 867250161-[2-(1,3-Dioxolan-2-yl)ethyl]-7-methoxy-4-methylquinolin-2(1H)one

생성물 1

HCID 867250173-(7-Methoxy-4-methyl-2-oxoquinolin-1(2H)-yl)propanal수율 74%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

To a solution of 1-[2-(1,3-dioxolan-2-yl)ethyl]-7-methoxy-4-methylquinolin-2(1H)one (30 ml) was added 4N hydrochloric acid (30 ml) and the mixture was stirred at room temperature for 2 hours. An aqueous solution of sodium carbonate/hydrogen carbonate was added to the reaction solution and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with water and saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure and the obtained crude product was purified by thin layer chromatography (hexane/ethyl acetate) to yield 630 mg (74%) of the title compound.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe obtained organic layer was washed with water and saturated sodium chloride solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe obtained crude product
  6. customwas purified by thin layer chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-2e1ce78b3d804bf9a251f969555f06fc
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952010B2

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