反应详情

8-Chlorotheophylline (20 g, 93.19 mmol) was dissolved in 800 ml of DMF and 2-cyanobenzyl bromide (18.28 g, 93.19 mmol), potassium carbonate (12.88 g, 93.19 mmol), and potassium iodide (10 mg, 0.06 mmol) were added. The mixture was stirred at room temperature for 20 hours. The solvent was evaporated and the residue was suspended in 900 ml of water and 900 ml of EtOAc, and compound (1A) was collected by filtration of the suspension. The layers in the mother liquor were separated and the aqueous layer was extracted with 3×500 ml of EtOAc. The combined organic layers were washed with 1×500 ml of water, and the solvent was evaporated to give compound (1A) as white crystals.

1. customThe solvent was evaporated
2. filtration900 ml of EtOAc, and compound (1A) was collected by filtration of the suspension
3. customThe layers in the mother liquor were separated
4. extractionthe aqueous layer was extracted with 3×500 ml of EtOAc
5. washThe combined organic layers were washed with 1×500 ml of water
6. customthe solvent was evaporated