反应详情

0.60 g (1.86 mmol) of 4-(4-methylsulfonylaminophenylsulfonyl)piperidine hydrochloride obtained in Example 5, 0.44 g (3.72 mmol) of 6-methyl-2-vinylpyridine and 0.31 g of sodium acetate were suspended in 10 ml of a mixture of methanol with water (1:1) and the suspension was refluxed for 2 h. The reaction liquid was filtered and the filtrate was concentrated to give a residue. After extraction with dichloromethane followed by washing with water, the organic layer was concentrated to precipitate white crystals. The crystals were collected by filtration and recrystallized from ethyl acetate to give 0.52 g (yield: 64%) of the intended compound.

1. temperaturethe suspension was refluxed for 2 h
2. customThe reaction liquid
3. filtrationwas filtered
4. concentrationthe filtrate was concentrated
5. customto give a residue
6. extractionAfter extraction with dichloromethane
7. washby washing with water
8. concentrationthe organic layer was concentrated
9. customto precipitate white crystals
10. filtrationThe crystals were collected by filtration
11. customrecrystallized from ethyl acetate