反应详情

Ethyl 3-{[6-(acetylamino)pyridin-3-yl]ethynyl}-4-methylbenzoate (0.68 mmol) in 5 ml of ethanol is cooled to 0° C. To this solution is dropped in 3 ml of 1M NaOH. The hydrolysis is stirred at this temperature for 2 h and r.t. for 3 h. The solvent (ethanol) is evaporated, and more water is added to dissolve the solid. The clear solution is washed with ether twice and then titrated with 2M HCl to pH 6. The precipitate is filtered, washed with water and ether, and dried to afford the product. The filtrate (pH 6) was extracted with DCM, dried, and evaporated to obtain additional amount of the hydrolyzed product.

1. customThe solvent (ethanol) is evaporated
2. additionmore water is added
3. dissolutionto dissolve the solid
4. washThe clear solution is washed with ether twice
5. filtrationThe precipitate is filtered
6. washwashed with water and ether
7. customdried
8. customto afford the product
9. extractionThe filtrate (pH 6) was extracted with DCM
10. customdried
11. customevaporated
12. customto obtain additional amount of the hydrolyzed product