反应详情

116 μl (1.49 mmol) of mesyl chloride are added, under a nitrogen atmosphere at a temperature of 5° C., to 0.473 g (1.36 mmol) of (1-aminoimidazo[1,5-a]pyridin-3-yl)(3-methoxy-4-nitrophenyl)methanone hydrochloride obtained in example 76 in 14 ml of pyridine. On completion of the introduction, the mixture is allowed to return to ambient temperature and is stirred for 30 minutes. The reaction medium is poured under 95 ml of 2N hydrochloric acid and extracted with ethyl acetate. The organic phase is washed with water, separated by settling, dried over sodium sulfate and concentrated under reduced pressure. The solid residue obtained is taken up in isopropyl ether, filtered off, washed with isopropyl ether and then dried. 0.40 g of an orange solid is collected. Melting point: 231° C.; 1H NMR (d6-DMSO): 3.24 (3H, s), 4.02 (3H, s), 7.40-7.44 (1H, m), 7.49-7.53 (1H, m), 7.88-7.92 (1H, d), 8.00-8.07 (2H, m), 8.26 (1H, s), 9.75 (1H, d)

1. customto return to ambient temperature
2. additionThe reaction medium is poured under 95 ml of 2N hydrochloric acid
3. extractionextracted with ethyl acetate
4. washThe organic phase is washed with water
5. customseparated
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe solid residue obtained
9. filtrationfiltered off
10. washwashed with isopropyl ether
11. customdried
12. custom0.40 g of an orange solid is collected