反应详情

温度

60 °C

In a 25 mL round-bottomed flask, 2-phenyl-2H-1,2,3-triazole-4-carboxylic acid (CAS 13306-99-5) (59.8 mg, 316 μmol, Eq: 1.1), (S)-tert-butyl 2-(4-aminophenyl)morpholine-4-carboxylate (80 mg, 287 μmol, Eq: 1.00), N-methylmorpholine (87.2 mg, 94.8 μl, 862 μmol, Eq: 3) and HBTU (164 mg, 431 μmol, Eq: 1.5) were combined with DMF (2 ml) to give a yellow solution. The reaction mixture was stirred overnight at 60° C. The mixture was poured into water (10 ml) and extracted twice with EtOAc. The organic layers were washed with NaHCO3, brine, dried over MgSO4, filtered and concentrated in vacuo to give a brown crude mixture. This mixture was diluted with ether, stirred for 15 minutes and the suspension was filtered. The resulting solid was washed several times with ether to afford the desired compound as a light-yellow solid (35 mg, 27.1%).

1. customto give a yellow solution
2. extractionextracted twice with EtOAc
3. washThe organic layers were washed with NaHCO3, brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customto give a brown crude mixture
8. stirringstirred for 15 minutes
9. filtrationthe suspension was filtered
10. washThe resulting solid was washed several times with ether