반응 #560437

반응 방정식

5-bromo-4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazole-3-thiol

ethyl 2-bromo-2-methylpropanoate

diisopropylethylamine

→

ethyl 2-(5-bromo-4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazol-3-ylthio)-2-methylpropanoate

수율 91.0%

용매

DMF

반응 조건

후처리

1. 1
   농축The mixture was then concentrated
2. 2
   기타sonicated in ethyl ether
3. 3
   workup.DISSOLUTIONuntil fully dissolved
4. 4
   세척washed with 1N HCl
5. 5
   추출The mixture was extracted with diethyl ether (2×5 mL)
6. 6
   건조the combined organic extracts dried over sodium sulfate
7. 7
   여과filtered
8. 8
   농축concentrated

실험 절차

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%).

출처