反应详情

7.100 g (approx. 10.92 mmol, purity 40%) of 3-iodo-6-methyl-1H-pyrazolo[3,4-d]pyrimidine and 4.626 g (14.20 mmol) of caesium carbonate were initially charged in 100 ml of DMF, and 2.939 g (14.20 mmol) of 2,3-difluorobenzyl bromide dissolved in 50 ml of DMF were added. The reaction mixture was stirred at RT for 3 h, added to 1.5 l of ice-water and extracted with diethyl ether. 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). 1.360 g of the target compound were obtained (31% of theory).

1. additionwere added
2. extractionextracted with diethyl ether
3. dry with materialThe organic phase was dried over sodium sulphate
4. concentrationconcentrated on a rotary evaporator
5. customThe residue was purified by means of preparative HPLC (eluent: acetonitrile/water, gradient 30:70→95:5)