反应详情

温度

65 °C

4-Methyl-3-(1-morpholinophthalazin-6-yl)benzoic acid (100 mg, 286 μmol) was dissolved in thionyl chloride (5.7 mL) and heated to 65° C. for 1 h before being concentrated in vacuo. The concentrate was dissolved in THF (5.7 mL), and DIPEA (150 μL, 859 μmol) and ethylamine—2 M in THF (0.71 mL) were added at 0° C. The reaction mixture was warmed to RT and stirred for 3 h, then diluted with 50 mL of ethyl acetate, added to a separation funnel, partitioned with sodium bicarbonate (saturated, aqueous), washed 3× with 50 mL of sodium bicarbonate (saturated, aqueous), separated, dried over sodium sulfate, and concentrated in vacuo to give a crude residue, which was purified by chromatography to afford the title compound. MS (ES+): 377(M+H)+.

1. concentrationbefore being concentrated in vacuo
2. dissolutionThe concentrate was dissolved in THF (5.7 mL)
3. temperatureThe reaction mixture was warmed to RT
4. additionadded to a separation funnel
5. custompartitioned with sodium bicarbonate (saturated, aqueous)
6. washwashed 3× with 50 mL of sodium bicarbonate (saturated, aqueous)
7. customseparated
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated in vacuo
10. customto give a crude residue, which
11. customwas purified by chromatography