反应详情

See FIG. 16(c). 1-((6-methoxy-5-methylpyrimidin-4-yl)methyl)-1H-pyrrolo[3,2-b]pyridine-3-carboxylic acid (250 mg, 0.84 mmol) was taken in a 100 ml single necked flask equipped with an air condenser connected to nitrogen source. DCM (10 mL) was added to get a suspension. Triethyl amine (1.162 mL, 8.38 mmol) was added to get a clear solution. 1-Propanephosphonic acid cyclic anhydride (1.497 mL, 2.51 mmol) was added followed by the addition of 2-fluoroethanamine hydrochloride (83 mg, 0.84 mmol). The reaction mass was stirred at RT for overnight, suspension was observed. After completion of the reaction, diluted with DCM, added water, and separated the DCM layer washed with brine solution. The DCM layer was dried over sodium sulphate, evaporated and purified the compound by column chromatography. Yield-52%. ES+MS m/z: 344 (M+1). 1H NMR (300 MHz, DMSO-d6) δ ppm 2.25 (s, 20 H) 3.67 (d, J=5.46 Hz, 7 H) 3.77 (d, J=5.46 Hz, 7 H) 4.50 (t, J=4.90 Hz, 7 H) 4.66 (t, J=4.99 Hz, 7 H) 5.69 (s, 13 H) 7.26 (dd, J=8.29, 4.71 Hz, 7 H) 7.94 (d, J=8.48 Hz, 7 H) 8.28 (s, 7 H) 8.41 (s, 6 H) 8.49 (d, J=4.52 Hz, 7 H) 8.95 (t, J=5.84 Hz, 7 H).

1. customequipped with an air condenser
2. customto get a suspension
3. customto get a clear solution
4. customAfter completion of the reaction
5. customseparated the DCM layer
6. washwashed with brine solution
7. dry with materialThe DCM layer was dried over sodium sulphate
8. customevaporated
9. custompurified the compound by column chromatography