反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred solution of 7-(4-fluoro-3-methoxyphenyl)-3-trifluoromethylimidazo[1,2-b][1,2,4]triazine (0.123 g, 0.397 mmol) in chloroform (5 ml) was added boron tribromide (1.19 ml, 1.91 mmol) and the mixture was stirred under nitrogen at room temperature for 21 h. 2 M NaOH (5 ml) was added and the mixture was stirred for 5 min producing a solid which was filtered and washed with water. The filtrate was washed with dichloromethane, and the aqueous layer was neutralised with concentrated hydrochloric acid causing a solid to precipitate. The solid was filtered, washed with water and dried under a vacuum to leave 109 mg (93%) of the title compound: 1H NMR (360 MHz, DMSO-d6) δ 7.38 (1H, dd, J 8.8, 11.2 Hz), 7.60-7.64 (1H, m), 7.88 (1H, dd, J 1.9, 8.6 Hz), 9.32 (1H, s), 10.26 (1H, s); MS (ES+) m/z 299 [M+H]+.
WORKUP
后处理
- stirringthe mixture was stirred for 5 min
- customproducing a solid which
- filtrationwas filtered
- washwashed with water
- washThe filtrate was washed with dichloromethane
- customto precipitate
- filtrationThe solid was filtered
- washwashed with water
- customdried under a vacuum