反应详情

温度

75 °C

To a solution of trans-N-(7-bromo-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]-oxazepin-1-yl)-2,2,2-trifluoroacetamide (0.5 g, 1.1 mmol) in DME (16 mL), Pd2(dba)3 (12.5 mg, 13.5 μmol), 2-(di-t-butyl-phosphino)biphenyl (25 mg, 80 μmol), sodium-tert-butoxide (218 mg, 2.3 mmol) and benzylamine (243 mg, 2.3 mmol) were added. The resulting reaction mixture was heated to 75° C. and stirred at this temperature for 48 h. The reaction mixture was quenched with sat NaHCO3 (aq) and extracted with ethyl acetate. The organic layer was washed with water and brine, dried (Na2SO4) and evaporated. The crude product was chromatographed with heptane/ethyl acetate 8:2 and purified with HPLC to afford the title compound (21 mg, 32%). Data: 1H-NMR (400 MHz, DMSO) 1.54-2.02 (m, 4H), 2.95 (t, J=9.2, 1H), 3.68 (d, J=14.0, 1H), 4.02 (d, J=10.0, 1H), 4.17 (d, J=6.0, 2H), 4.37 (m, 1H), 5.90-7.33 (12 ArH, 1 NH), 9.11 (d, J=10.0, 1H). (m/z)=468 (M+H)+.

1. customThe resulting reaction mixture
2. customThe reaction mixture was quenched with sat NaHCO3 (aq)
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with water and brine
5. dry with materialdried (Na2SO4)
6. customevaporated
7. customThe crude product was chromatographed with heptane/ethyl acetate 8:2
8. custompurified with HPLC