反应详情

Methyl 6-(6-chloro-2-methyl-3-oxo-2,3-dihydropyridazin-4-ylamino)nicotinate (1.523 g, 5.17 mmol, Eq: 1.00) was suspended in dioxane (90 ml). 1 M Lithium hydroxide (10.3 ml, 10.3 mmol, Eq: 2) was added dropwise. The light brown suspension was stirred overnight at room temperature. 1 M Lithium hydroxide (10.3 ml, 10.3 mmol, Eq: 2) was added again and stirred over the weekend. A mixture of ethyl acetate/ammonium chloride solution was added to the reaction mixture. The resulting precipitate was collected by filtration. The precipitate was triturated with water (200 ml), filtered, washed with ethyl acetate and dried in vacuo to give a light yellow solid (1.13 g). (M+H)+=278.8 m/e

1. stirringstirred over the weekend
2. additionwas added to the reaction mixture
3. filtrationThe resulting precipitate was collected by filtration
4. customThe precipitate was triturated with water (200 ml)
5. filtrationfiltered
6. washwashed with ethyl acetate
7. customdried in vacuo