m-Chloroperbenzoic acid → HCID 21287983、化合物
反応式
[Cl:1][CH:2]([CH2:7][C:8]1[CH:9]=[N:10][C:11]([S:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:12][CH:13]=1)[C:3]([O:5][CH3:6])=[O:4].ClC1C=CC=C(C(OO)=[O:29])C=1>ClCCl>[Cl:1][CH:2]([CH2:7][C:8]1[CH:9]=[N:10][C:11]([S:14]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[O:29])=[CH:12][CH:13]=1)[C:3]([O:5][CH3:6])=[O:4]参加物
4
実験手順
Methyl 2-chloro-3-(6-phenylthio-3-pyridyl)propionate (10.5 g), prepared in substantially the same manner as in Reference Example 5 using the corresponding starting materials, is dissolved in 100 ml of dichloromethane. To the solution, 7.1 g of m-chloroperbenzoic acid is added slowly with stirring under cooling in an ice-water bath. The mixture is stirred at room temperature for 1 hour, washed with saturated sodium carbonate solution, dried over magnesium sulfate, and concentrated to give crude methyl 2-chloro-3-(6-phenylsulfinyl-3-pyridyl)propionate. To the sulfinyl compound is added 170 ml of 4N sodium hydroxide solution, and the mixture is refluxed with stirring for 4 hours. After cooling, the resulting precipitate is collected to give 4.1 g of the title compound.