反应详情

温度

110 °C

A mixture of 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (100 mg, 0.67 mmol), 3-(4-amino-1,2,3-triazol-1-yl)pyrrolidine dihydrochloride (185 mg, 0.83 mmol) and diazabicycloundecane (127 mg, 0.83 mmol) in pyridine (3 ml) was heated at 110° C. for 24 hrs. Reaction mixture was concentrated to dryness under vacuum and residue was dissolved in water, extracted with methylene chloride, dried over sodium sulfate and concentrated to dryness. The solid residue thus obtained was crystallized from chloroform to brown solid. Yield 15 mg (10.4%), m.p. 210°-213° C. 1H NMR (TFA) δ: 1.22-1.58 (m, 4H), 2.70-2.90 (m, 2H), 4.06-4.54 (m, 5H), 5.48-5.60 (m, 1H), 7.79 (s, 1H), 9.14 (s, 1H).

1. customReaction mixture
2. concentrationwas concentrated to dryness under vacuum and residue
3. dissolutionwas dissolved in water
4. extractionextracted with methylene chloride
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated to dryness
7. customThe solid residue thus obtained
8. customwas crystallized from chloroform to brown solid