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Methanol → HCID 23017958, 화합물

HRID 1788398
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HRID 1788398 반응식
S(=O)(=O)(O)O.[F:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[N:15]=[C:14]([CH3:17])[CH:13]=[CH:12]2.[NH4+].[NH4+].[O-]S(OOS([O-])(=O)=O)(=O)=O.[OH2:30].[CH3:31]O>>[F:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[N:15]=[C:14]([CH3:17])[CH:13]=[C:12]2[CH2:31][OH:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 887MethanolHCID 962WaterHCID 1118Sulfuric AcidHCID 62648Ammonium PersulfateHCID 112406548-Fluoro-2-methylquinoline

생성물 1

HCID 23017958HCID 23017958, 화합물수율 32%

실험 절차

Concentrated sulfuric acid (1.2 mL) was added to a solution of 2.70 g (16.8 mmol) of 8-fluoro-2-methylquinoline and 7.70 g (33.7 mmol) of ammonium peroxodisulfate in a mixture of methanol (35 mL)-water (25 mL) and heated under reflux for 15 hours. The reaction mixture was left to cool, followed by a removal of methanol under a reduced pressure. Sodium carbonate was added to the residue to adjust its pH to 10, and then the mixture was extracted with chloroform. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, and the solvent was removed. The obtained residue was washed with ether to obtain 1.03 g (yield 32%) of (8-fluoro-2-methylquinolin-4-yl)methanol. Its physical properties are shown below.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 15 hours
  3. waitThe reaction mixture was left
  4. temperatureto cool
  5. customfollowed by a removal of methanol under a reduced pressure
  6. additionSodium carbonate was added to the residue
  7. extractionthe mixture was extracted with chloroform
  8. washThe organic layer was washed with saturated brine
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customthe solvent was removed
  11. washThe obtained residue was washed with ether

출처 및 근거

ORD 기록
ord-7b407a8250b7486dbbb86d1adc1d85a8
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07511144B2

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