HRID457695
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
To a solution of 2-benzylamino-9-ethyl-9H-purin-6-ylamine (1.0 mmol), a compound of formula (4), in 10 mL of dry DMF was added N-bromosuccinimide (267 mg, 1.5 mmol). The reaction mixture was stirred at room temperature for 1 hour. The solvent was then removed in vacuo and the residue partitioned between water and chloroform. The organic layer was washed with 1N sodium hydroxide, dried (Na2SO4), filtered, and the filtrate concentrated in vacuo. The residue was chromatographed on a silica gel column, eluting with chloroform/methanol; (98/2), to give 2-benzylamino-8-bromo-9-ethyl-9H-purin-6-ylamine as a chromatographically pure solid.
WORKUP
后处理
- customThe solvent was then removed in vacuo
- customthe residue partitioned between water and chloroform
- washThe organic layer was washed with 1N sodium hydroxide
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationthe filtrate concentrated in vacuo
- customThe residue was chromatographed on a silica gel column
- washeluting with chloroform/methanol