反应详情

温度

100 °C

To a 150 mL pressure vessel was added 5-(2-bromo-4-fluorophenyl)-2-(1-hydroxyethylidene)cyclohexane-1,3-dione (1E, 1.12 g, 3.42 mmol, 1.0 eq.), EtOH (30 mL), guanidine hydrochloride (818 mg, 8.56 mmol, 2.5 eq.), and dimethylamine (2.0 M in THF, 10 mL, 20.5 mmol, 6.0 eq.). The vessel was sealed and heated for 72 hours at 100° C. LC/MS determined the reaction to be complete. The reaction was cooled and concentrated to give a pasty gray solid. EtOH (−10 mL) was added to the residue and sonicated to give a suspension. The solid was collected by filtration and rinsed with cold EtOH to give a light-yellow solid (288 mg, 24%). ESI-MS: m/z 350.2 (M+H)+.

1. customThe vessel was sealed
2. customthe reaction
3. temperatureThe reaction was cooled
4. concentrationconcentrated
5. customto give a pasty gray solid
6. customsonicated
7. customto give a suspension
8. filtrationThe solid was collected by filtration
9. washrinsed with cold EtOH