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. The reaction was then concentrated in vacuo, dissolved in tetrahydrofuran 99.9% (5.7 mL) and diisopropylethylamine (150 μL, 859 μmol) and methylamine, 2.0 m solution in THF (0.7 mL) were added. The reaction mixture was stirred for 3 h at ambient temperature. The reaction mixture was diluted with 50 mL of EtOAc, added to an addition funnel and partitioned with sodium bicarbonate (saturated, aqueous). The organic layers were washed 3 times with 50 mL of sodium bicarbonate (saturated, aqueous), dried over sodium sulfate, and concentrated via rotovap to give a crude product. After purification by chromatography, the title compound was obtained. Found MS (ES+): 363(M+H)+.

1. concentrationThe reaction was then concentrated in vacuo
2. dissolutiondissolved in tetrahydrofuran 99.9% (5.7 mL)
3. additionadded to an addition funnel
4. custompartitioned with sodium bicarbonate (saturated, aqueous)
5. washThe organic layers were washed 3 times with 50 mL of sodium bicarbonate (saturated, aqueous)
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated via rotovap
8. customto give a crude product
9. customAfter purification by chromatography