反应 #1565194
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08349865B2
反应条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 1,5-dichloro-9-fluorobenzo[c]-2,6-naphthyridine (50 mg, 0.19 mmol) (Example 1, Step 5) in THF (3 mL), were added (2S)-1,1,1-trifluoro-3-methylbutan-2-amine (26 mg, 0.19 mmol) and lithium bis(trimethylsilyl)amide (0.56 mL, 1.0 M in THF, 0.56 mmol). The solution was heated to 85° C. for 1 hr then cooled to room temperature. The reaction mixture was quenched with methanol and concentrated under reduced pressure. The crude mixture was taken up in THF (1 mL) and HCl (1 mL, 6 N) and heated to 85° C. for 1.5 hr. The solution was cooled and worked up with EtOAc and saturated NaHCO3. The organic layers were combined, dried over MgSO4, filtered, and concentrated to afford the title product. then cooled to room temperature The reaction mixture was quenched with methanol concentrated under reduced pressure HCl (1 mL, 6 N) and heated to 85° C. for 1.5 hr The solution was cooled dried over MgSO4 filtered concentrated
来源 ID: ord-6bb31a79af52489f8d4fa5e12f06d6b7