HRID241035

反应详情

EQUATION

反应方程式

HRID 241035 的结构方程式

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of dimethylamine (2M solution in tetrahydrofuran, 40.0 mL, 80.0 mmol) was added 2-(chloromethyl)-7-(methyloxy)quinazolin-4-ol hydrochloride (7.5 g, 29 mmol) and the reaction mixture was stirred for 90 minutes at 50° C. After cooling it to room temperature the reaction mixture was concentrated and the residue was partitioned between water (100 mL) and ethyl acetate (250 mL). The organic layer was separated and washed with water (100 mL), saturated sodium bicarbonate (100 mL) and brine (100 mL), dried over sodium sulfate, filtered and concentrated to give 2-[(dimethylamino)methyl]-7-(methyloxy)quinazolin-4-ol (6.6 g, 97%). MS (EI) for C12H15N3O2: 234 (MH+).

WORKUP

后处理

  1. temperatureAfter cooling it to room temperature the reaction mixture
  2. concentrationwas concentrated
  3. customthe residue was partitioned between water (100 mL) and ethyl acetate (250 mL)
  4. customThe organic layer was separated
  5. washwashed with water (100 mL), saturated sodium bicarbonate (100 mL) and brine (100 mL)
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated