反应详情

15.45 g of 3-(1H pyrazol-3-yl)-pyridine prepared as indicated in CA 68 P 95812 g (1968) is introduced dropwise over 1 hour while maintaining the temperature below 30° C. or equal to 30° C. into a mixture of 20 ml of DMF and 6.13 g of sodium hydride. A solution of 29.90 g of 2-(4-bromobutyl)-1H -isoindole-1,3(2H)-dione and 110 ml of DMF is added dropwise. The reaction medium is agitated for 30 minutes at ambient temperature, followed by concentrating, pouring into 300 ml of water cooled down to 10° C., extracting with ethyl acetate, washing with water, drying, filtering and concentrating. The residue is taken up in methylene chloride, followed by drying, filtering and concentrating. 35.87 of a product is obtained which is crystallized from ethyl ether, dried, washed with water and dried. 22.93 g of sought product is obtained.

1. additionis introduced dropwise over 1 hour
2. temperaturewhile maintaining the temperature below 30° C.
3. concentrationby concentrating
4. additionpouring into 300 ml of water
5. temperaturecooled down to 10° C.
6. extractionextracting with ethyl acetate
7. washwashing with water
8. customdrying
9. filtrationfiltering
10. concentrationconcentrating
11. customby drying
12. filtrationfiltering
13. concentrationconcentrating
14. custom35.87 of a product is obtained which
15. customis crystallized from ethyl ether
16. customdried
17. washwashed with water
18. customdried