反应详情

温度

110 °C

First, 8.20 g (115 mmol) of crotonaldehyde and 9.55 g (57.2 mmol) of benzenesulfonyl cyanide were introduced to the same reaction vessel as in Example 1. Toluene (15 ml) was added as the solvent, and 1.33 g (5.78 mmol) of tributyl borate was added. Then the mixture was heated under reflux for 3 hours while agitating at an internal temperature of 110° C. in a nitrogen atmosphere, separating and removing water that was produced. After this solution was cooled to room temperature, the low-boiling components, such as solvent, etc., were removed under reduced pressure and the resulting concentrate was cooled in an ice bath to precipitate crystals. The crystals were filtered with a glass filter and washed with 10 ml of toluene that had been cooled to 5° C. or lower. Then the crystals were dried for 2 hours in vacuo to give 10.9 g of 2-benzenesulfonylpyridine as colorless crystals (purity of 98%, yield of 85% based on benzenesulfonyl cyanide).

1. additionwas added
2. temperatureThen the mixture was heated
3. temperatureunder reflux for 3 hours
4. customseparating
5. customremoving water that
6. customwas produced
7. temperatureAfter this solution was cooled to room temperature
8. customthe low-boiling components, such as solvent, etc., were removed under reduced pressure
9. concentrationthe resulting concentrate
10. temperaturewas cooled in an ice bath
11. customto precipitate crystals
12. filtrationThe crystals were filtered with a glass
13. filtrationfilter
14. washwashed with 10 ml of toluene that
15. temperaturehad been cooled to 5° C.
16. customThen the crystals were dried for 2 hours in vacuo