反应详情

温度

160 °C

To a 3 mL microwave vial was added 3-((4S,6S)-2-benzamido-4-(fluoromethyl)-6-(trifluoromethyl)-5,6-dihydro-4H-1,3-oxazin-4-yl)-4-fluorobenzoic acid (76.5 mg, 0.17 mmol). 2-amino-5-chlorophenol (74.0 mg, 0.52 mmol) and polyphosphoric acid (0.50 mL). The mixture was purged with Ar for 1 min, then the tube was sealed and heated to 160° C. for 1 h. The mixture was then diluted with Na2CO3 in water and extracted with DCM three times. The organic layer was dried over Na2SO4, and concentrated in vacuo. The crude was purified by reverse phase HPLC: 10-100% in 26 min, MeCN in water with 0.1% TFA. The combined fractions were neutralized with solid Na2CO3, and extracted with DCM three times. The organic phase was dried over Na2SO4 and concentrated in vacuo. The product was obtained as an off-white solid (2.6 mg, 3.6% yield). MS m/z=446 [M+H]+. Calculated for C19H13ClF5N3O2: 445.8.

1. customThe mixture was purged with Ar for 1 min
2. customthe tube was sealed
3. additionThe mixture was then diluted with Na2CO3 in water
4. extractionextracted with DCM three times
5. dry with materialThe organic layer was dried over Na2SO4
6. concentrationconcentrated in vacuo
7. customThe crude was purified by reverse phase HPLC
8. extractionextracted with DCM three times
9. dry with materialThe organic phase was dried over Na2SO4
10. concentrationconcentrated in vacuo