反应详情

A solution of 5-bromo-4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazole-3-thiol (50 mg, 0.144 mmol), ethyl 2-bromo-2-methylpropanoate (22 μL, 0.144 mmol) and diisopropylethylamine (76 μL, 0.433 mmol) in DMF (1 mL) was heated to 60° C. for 20 hours. The mixture was then concentrated, sonicated in ethyl ether until fully dissolved, and washed with 1N HCl. The mixture was extracted with diethyl ether (2×5 mL), and the combined organic extracts dried over sodium sulfate, filtered, and concentrated to provide ethyl 2-(5-bromo-4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazol-3-ylthio)-2-methylpropanoate as a brown oil (60 mg, 91%).

1. concentrationThe mixture was then concentrated
2. customsonicated in ethyl ether
3. dissolutionuntil fully dissolved
4. washwashed with 1N HCl
5. extractionThe mixture was extracted with diethyl ether (2×5 mL)
6. dry with materialthe combined organic extracts dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated