HRID916776
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
(Bromomethyl)cyclopropane (7.6 mL, 78 mmol) was added to a solution of 4-Chloro-7H-pyrrolo[2,3-d]pyrimidine (10.0 g, 65 mmol) and cesium carbonate (25.4 g, 78 mmol) in DMF (100 mL). The reaction mixture was stirred at room temperature 12 h, filtered, and concentrated in vacuo. Purification by flash column chromatography (silica, 1:9→2:8 EtOAc:hexanes) provided the title compound as a white solid (12.9 g, 95%). MS: 208.5 (MH+); HPLC Rf: 5.21 min. (HPLC method 4); HPLC purity: 100%.
WORKUP
后处理
- filtrationfiltered
- concentrationconcentrated in vacuo
- customPurification by flash column chromatography (silica, 1:9→2:8 EtOAc:hexanes)