HRID356651
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
9.2 g of 4-[4-chloro-5-(2-chloro-5-methoxy-phenoxy )-6-methyl-pyrimidin-2-yl]-morpholine and 17.8 g of 5-isopropyl-pyridine-2-sulphonamide potassium in 130 ml of dry dimethyl sulphoxide were heated to 120° C. under argon for 16 hours. Thereafter, the dimethyl sulphoxide was distilled off, the residue was partitioned between ethyl acetate and 1 N hydrochloric acid and the organic phase was washed neutral. The organic phase was dried, the solvent was evaporated and the residue was recrystallized from ethanol. 10.3 g of 5-isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy )-6-methyl-2-morpholin-4-yl-pyrimidin-4-ylamide, MS: M =534, were obtained.
WORKUP
后处理
- distillationThereafter, the dimethyl sulphoxide was distilled off
- customthe residue was partitioned between ethyl acetate and 1 N hydrochloric acid
- washthe organic phase was washed neutral
- customThe organic phase was dried
- customthe solvent was evaporated
- customthe residue was recrystallized from ethanol