反应详情

温度

45 °C

To a solution of 8.98 g (86.33 mmole) sodium bisulfite in water (27 mL), o-chlorobenzaldehyde 12.4 g (86.33 mmole) was added resulting in a white precipitate. To the precipitate, 15 g (0.107 moles) of 6,7-dihydro-4H-thieno[3,2-c]pyridine was added, followed by addition of 4.4 g (89.7 mmoles) NaCN (dissolved in 15 mL water). The reaction mixture was heated at 40-50° C. for 6 hrs and was quenched by pouring in water (50 mL). The mixture was extracted with 2×100 mL of ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure. The yield of the title product is 24 g (97%).

1. customresulting in a white precipitate
2. customwas quenched
3. additionby pouring in water (50 mL)
4. extractionThe mixture was extracted with 2×100 mL of ethyl acetate
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. customthe solvent was removed under reduced pressure