Methanol → HCID 23017958、化合物

反応式

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]

参加物

反応物 5

HCID 887Methanol

HCID 962Water

HCID 1118Sulfuric Acid

HCID 62648Ammonium Persulfate

HCID 112406548-Fluoro-2-methylquinoline

生成物 1

HCID 23017958HCID 23017958、化合物収率 32%

実験手順

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.