反应详情

温度

60 °C

A solution of potassium hydroxide (18.7 ml, 18.7 mmol) in methanol and hydroxylamine hydrochloride (18.7 ml, 18.7 mmol) in methanol were mixed, filtered and added to 2-(2-bromo-4-fluorophenyl)acetonitrile (1 g, 4.67 mmol) in MeOH and stirred at 60° C. for 24 h, evaporated to dryness. The residue was dissolved in chloroform (30.0 ml) and to this was added dimethyl but-2-ynedioate (730 mg, 5.14 mmol). The mixture was stirred at 60° C. for 24 h, cooled and evaporated to dryness. The residue was dissolved in xylene (10 ml) and heated at 120° C. for 2 h in microwave oven. The cooled residue was evaporated to dryness and then triturated with EtOAc, filtered and washed with Et2O to give the title compound as a brown solid (0.21 g; 12%). LCMS: m/z=358 (MH+).

1. filtrationfiltered
2. customevaporated to dryness
3. dissolutionThe residue was dissolved in chloroform (30.0 ml)
4. stirringThe mixture was stirred at 60° C. for 24 h
5. temperaturecooled
6. customevaporated to dryness
7. dissolutionThe residue was dissolved in xylene (10 ml)
8. temperatureheated at 120° C. for 2 h in microwave oven
9. customThe cooled residue was evaporated to dryness
10. customtriturated with EtOAc
11. filtrationfiltered
12. washwashed with Et2O