反应详情

温度

100 °C

A mixture of ethyl 6-[(5-chloro-2-{[(4-chloro-2-fluorophenyl)methyl]oxy}-phenyl)methyl]-2-pyridinecarboxylate (453 mg), sodium thiomethoxide (370 mg) and dimethylformamide (5 ml) was stirred at 100° C. for 2.5 hours. After cooling water (30 ml) was added and the mixture extracted with ethyl acetate (2×25 ml). The aqueous layer was acidified with conc. hydrochloric acid and extracted with ethyl acetate (2×25 ml). The combined extracts were washed with water (10 ml), dried (MgSO4) and concentrated in vacuo. The residue was washed with water and recrystallised from ether to afford the title compound (208 mg, 76%) as a pale buff solid.

1. additionwas added
2. extractionthe mixture extracted with ethyl acetate (2×25 ml)
3. extractionextracted with ethyl acetate (2×25 ml)
4. washThe combined extracts were washed with water (10 ml)
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. washThe residue was washed with water
8. customrecrystallised from ether