HRID2079645
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
A 0.15M suspension of 4-(6-bromo-7-methoxyquinazolin-2-ylamino)-N-isopropylbenzamide (1.0 eq) and sodium thiomethoxide (4.0 eq) in DMF was heated to 80° C. in an oil bath for 12 h. The mixture was partitioned between ethyl acetate and water. The pH of aqueous phase was adjusted to 5 by adding saturated ammonium hydrochloride. Aqueous phase was extracted with ethyl acetate, and combined organic phase was washed with brine, dried over sodium sulfate, and concentrated to give desired product in 90% yield. ES/MS m/z 401/403 (MH+).
WORKUP
后处理
- customThe mixture was partitioned between ethyl acetate and water
- additionby adding saturated ammonium hydrochloride
- extractionAqueous phase was extracted with ethyl acetate, and combined organic phase
- washwas washed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated