反应详情

5-(2,4-dimethoxy-benzyl)-3-(4-fluoro-phenyl)-7-oxo-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine-6-carboxylic acid methyl ester (0.39 g, 0.86 mmol), example 31-e, was dissolved in 6 mL of anhydrous dichloromethane. To the solution was added 93.7 μL of thionyl chloride, and the reaction mixture was stirred for 5 hours. The solution was filtered on a fine glass frit filter to collect a white solid precipitate. The solid was washed twice with cold dichloromethane and then partitioned between saturated sodium bicarbonate solution and ethyl acetate. The organic fraction was washed with brine, dried over anhydrous sodium sulfate, and concentrated to produce 0.16 g of a white solid. MS: (+) m/z 304.0 (M+1)

1. filtrationThe solution was filtered on a fine glass frit
2. filtrationfilter
3. customto collect a white solid precipitate
4. washThe solid was washed twice with cold dichloromethane
5. custompartitioned between saturated sodium bicarbonate solution and ethyl acetate
6. washThe organic fraction was washed with brine
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated