反应详情

To a solution of 4-methylpyrazole (10.5 mg, 0.13 mmol) in DMA (0.65 mL) in a microwave vial was added Cs2CO3 (83 mg, 0.26 mmol) and the mixture was stirred at rt. After 15 min, Intermediate 3 (40 mg, 0.13 mmol) was added and the tube was capped, sealed, and heated at 150° C. for 3 h. The reaction was cooled to rt, filtered through a syringe filter and purified by reverse-phase preparative chromatography (5-50% acetonitrile/water+0.1% TFA) to give Example 2. 1H NMR: (500 MHz, CD3OD) δ 8.31 (m, 1H), 7.76 (m, 1H), 7.54 (m, 1H), 7.33 (m, 3H), 6.62 (s, 1H), 4.64 (m, 4H), 4.31 (m, 1H), 3.73 (s, 3H), 2.51 (s, 3H), 2.14 (s, 3H) ppm. MS: m/z=360.5 (M+H).

1. customthe tube was capped
2. customsealed
3. temperatureheated at 150° C. for 3 h
4. temperatureThe reaction was cooled to rt
5. filtrationfiltered through a syringe
6. filtrationfilter
7. custompurified by reverse-phase preparative chromatography (5-50% acetonitrile/water+0.1% TFA)
8. customto give Example 2