HRID408475

反应详情

EQUATION

反应方程式

HRID 408475 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvents were removed under reduced pressure
  2. dissolutionThe residue was dissolved in ethyl acetate (150 mL)
  3. washwashed with NaHCO3, brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customto give crude product, which
  8. customwas purified by column (ethyl acetate:hexanes=1:2)