HRID1527723
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 10 mL round-bottomed flask were added a stir bar, ethyl 3-(1-(4-bromobenzyl)-6-hydroxy-1H-benzo[d]imidazol-2-yl)-2,2-dimethylpropanoate (100 mg, 0.23 mmol), cesium carbonate (227 mg, 0.69 mmol), DMF (2 mL), and 2-(chloromethyl)-5-methylpyridine hydrochloride salt (41 mg, 0.23 mmol). After 12 h, the mixture was partitioned between water (50 mL) and EtOAc (20 mL). The organic layer was separated and the aqueous layer was further extracted with EtOAc (2×20 mL). The combine organic layers were dried with sodium sulfate, filtered, and concentrated to dryness (124 mg, 99%). MS (ESI): mass calcd. for C28H30BrN3O3, 535.15; m/z found, 536.1 [M+H]+.
WORKUP
后处理
- additionTo a 10 mL round-bottomed flask were added a stir bar
- customthe mixture was partitioned between water (50 mL) and EtOAc (20 mL)
- customThe organic layer was separated
- extractionthe aqueous layer was further extracted with EtOAc (2×20 mL)
- dry with materialThe combine organic layers were dried with sodium sulfate
- filtrationfiltered
- concentrationconcentrated to dryness (124 mg, 99%)