反应详情

A suspension of 70.25 mg (0.25 mmol) of (-) -9,10-difluoro-3(S)-methyl-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de]-1,4-benzoxazine-6-carboxylic acid and 87 mg (0.5 mmol) of 3-(1,2,4-triazol-1-yl)pyrrolidine hydrochloride in 3 ml of acetonitrile in the presence of 76 mg (0.5 mmol) DBU was stirred under nitrogen at reflux condition overnight. The yellow solution was then evaporated to dryness and to the residue, water was added and solid collected. The off-white solid was dissolved in chloroform and the small amounts of the suspension were filtered off. The supernatant was evaporated and to the residue, water was added and solid collected (60 mg), m.p. 229°-231° C. 1H NMR (CDCl3) δ: 8.59 (s, 1H), 8.26 (s, 1H), 7.98 (s, 1H), 7.7 (d, 13.5Hz, 1H), 5.17-5.00 (m, 1H), 4.6-3.73 (m, 7H), 2.67-2.4 (m, 2H), 1.61 (d, 6.7Hz, 3H).

1. temperatureat reflux condition overnight
2. customThe yellow solution was then evaporated to dryness and to the residue, water
3. additionwas added
4. customsolid collected
5. dissolutionThe off-white solid was dissolved in chloroform
6. filtrationthe small amounts of the suspension were filtered off
7. customThe supernatant was evaporated and to the residue, water
8. additionwas added
9. customsolid collected (60 mg), m.p. 229°-231° C