反应详情

A solution of 4-(5-(4-methoxyphenyl)-1-methyl-1H-1,2,3-triazol-4-yl)pyridine (170 mg, 0.64 mmol) in dichloromethane (5 mL) was treated at RT With boron tribromide (1.27 mL of 1M in dichloromethane) and the mixture was stirred overnight. Aqueous 1N NaOH (10 mL) was added, and after being stirred 1 h the mixture was extracted with dichloromethane (20 mL). The aqueous layer was acidified to pH 7 with 2N HCl, and extracted with ethyl acetate (2×15 mL). The extracts were dried with sodium sulfate and concentrated giving a yellow solid (142 mg, 88%). 1H NMR (CDCl3, 400 mHz) δ 1H NMR (CDCl3, 400 mHz) δ 8.39 (d, 2H, J=5-6 Hz), 7.49 (d, 2H, J=5-6 Hz), 7.09 (d, 2H, J=8.7 Hz), 6.95 (d, 2H, J=8.7 Hz), 3.87 (s, 3H). MS (AP−) 351 (M−H).

1. stirringafter being stirred 1 h the mixture
2. extractionwas extracted with dichloromethane (20 mL)
3. extractionextracted with ethyl acetate (2×15 mL)
4. dry with materialThe extracts were dried with sodium sulfate
5. concentrationconcentrated