HRID2353653
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
(4-{4-Morpholin-4-yl-6-[(phenylsulfonyl)methyl]pyrimidin-2-yl}phenyl)amine (1 g, 2.44 mmol) was dissolved in dioxane (10 mL). Sodium bicarbonate (307 mg, 3.65 mmol) was added, followed by phenyl chloroformate (0.307 mL, 2.44 mmol) and the reaction stirred at room temperature for 2 hours. The solvent was removed in vacuo, and the resultant oil partitioned between 10 mL DCM and 10 mL water. The organic phase was dried over magnesium sulphate, filtered and concentrated in vacuo. The cream solid obtained was chromatographed on silica, eluting with 0-50% ethyl acetate in DCM, to give the desired material as a white solid (790 mg).
WORKUP
后处理
- customThe solvent was removed in vacuo
- customthe resultant oil partitioned between 10 mL DCM and 10 mL water
- dry with materialThe organic phase was dried over magnesium sulphate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe cream solid obtained
- customwas chromatographed on silica
- washeluting with 0-50% ethyl acetate in DCM