HRID570525
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
7.950 g (13.76 mmol) of 3-iodo-6-methyl-1H-pyrazolo[3,4-d]pyrimidine and 4.930 g (15.13 mmol) of caesium carbonate were initially charged in 20 ml of DMF, and 2.860 g (15.13 mmol) of 2-fluorobenzyl bromide dissolved in 5 ml of DMF were added. The reaction mixture was stirred at RT overnight, diluted with 100 ml of water and extracted with ethyl acetate. The organic phase was dried over sodium sulphate and concentrated on a rotary evaporator. The residue was purified by means of preparative HPLC (eluent: acetonitrile/water, gradient 30:70→95:5). 1.030 g of the target compound were obtained (20% of theory).
WORKUP
后处理
- additionwere added
- extractionextracted with ethyl acetate
- dry with materialThe organic phase was dried over sodium sulphate
- concentrationconcentrated on a rotary evaporator
- customThe residue was purified by means of preparative HPLC (eluent: acetonitrile/water, gradient 30:70→95:5)