[CH2:1]([O:3][C:4]([C:6]1[S:10][C:9](SC)=[N:8][C:7]=1[NH2:13])=[O:5])[CH3:2].[CH3:14]O.O[O:17][S:18]([O-:20])=O.[K+]>O.C(OCC)(=O)C>[CH2:1]([O:3][C:4]([C:6]1[S:10][C:9]([S:18]([CH3:14])(=[O:20])=[O:17])=[N:8][C:7]=1[NH2:13])=[O:5])[CH3:2]After adding 41.8 g of 4-amino-2-methylsulfanylthiazole-5-carboxylic acid ethyl ester [CAS No. 39736-29-3] to 3 liters of a water:methanol=1:1 mixed solvent at room temperature, 352 g of Oxone™ was added thereto in small portions over a period of 15 minutes with stirring. The mixture was stirred at room temperature for 16 hours and then poured into a mixture of 8 liters of ethyl acetate and 5 liters of water. The organic layer was washed with 5 liters of water and 3 liters of saturated brine and then dried over anhydrous magnesium sulfate. The desiccating agent was removed by filtration, and the filtrate was concentrated under reduced pressure to give the title compound (34.5 g) as a light yellow solid.
読み込み中…
