HRID2189796
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Ethyl 3-(4-cyano-1H-indazol-1-yl)-2,2-dimethylpropanoate (D102) (348 mg, 1.28 mmol), hydroxylamine hydrochloride (1.087 g, 10.26 mmol), NaHCO3 (1.078 g, 12.83 mmol) in MeOH (20 ml) was heated at 65° C. for 24 h then at room temperature over the weekend. The mixture was filtered, concentrated, treated with water and vigorously stirred for 10 mins, filtered and dried to give a colourless solid, dried overnight in vacuo at 45° C. to give the title compound (373 mg, 90%). MS (ES) C15H20N4O3 requires 304, found 305 [M+H]+
WORKUP
后处理
- customat room temperature
- filtrationThe mixture was filtered
- concentrationconcentrated
- additiontreated with water
- filtrationfiltered
- customdried
- customto give a colourless solid
- customdried overnight in vacuo at 45° C.