HRID241076

反应详情

EQUATION

反应方程式

HRID 241076 的结构方程式

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of dimethylamine (2M solution in tetrahydrofuran, 4.0 mL, 8.0 mmol) was added 2-(1-chloroethyl)-6,6-dimethyl-5,6,7,8-tetrahydroquinazolin-4-ol (synthesized according to the method of reagent preparation 18 using 2-chloropropionitrile in step 1) (50 mg, 0.21 mmol) and the reaction mixture was stirred in a sealed tube for 16 hours at 80° C. After cooling to room temperature the reaction mixture was concentrated and the residue was partitioned between brine (50 mL) and ethyl acetate (50 mL). The organic layer was separated and washed with brine (20 mL), dried over sodium sulfate, filtered and concentrated to give 2-[1-(dimethylamino)ethyl]-6,6-dimethyl-5,6,7,8-tetrahydroquinazolin-4-ol (50 mg, 96%). MS (EI) for C14H23N3O: 250 (MH+).

WORKUP

后处理

  1. customsynthesized
  2. temperatureAfter cooling to room temperature the reaction mixture
  3. concentrationwas concentrated
  4. customthe residue was partitioned between brine (50 mL) and ethyl acetate (50 mL)
  5. customThe organic layer was separated
  6. washwashed with brine (20 mL)
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated