HRID408475
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 solution of the 2-(2,6-difluorophenyl)-8-methoxyquinazoline (1.0 eq) in methylene chloride (0.23M) was added BBr3 (2.0 eq) at room temperature. The reaction mixture was stirred overnight. The solvents were removed under reduced pressure. The residue was dissolved in ethyl acetate (150 mL), and washed with NaHCO3, brine, then dried over MgSO4, filtered, and evaporated under reduced pressure to give crude product, which was purified by column (ethyl acetate:hexanes=1:2) to yield 2-(2,6-difluorophenyl)quinazolin-8-ol (94%). LC/MS (m/z): 259.0 (MH+), Rt=0.82.
WORKUP
后处理
- customThe solvents were removed under reduced pressure
- dissolutionThe residue was dissolved in ethyl acetate (150 mL)
- washwashed with NaHCO3, brine
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated under reduced pressure
- customto give crude product, which
- customwas purified by column (ethyl acetate:hexanes=1:2)