HRID1091926

反应详情

EQUATION

反应方程式

HRID 1091926 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a flask containing 2,4-dichloro-5-chloromethyl-6-methyl-pyrimidine (107 mg, 0.51 mmol) in absolute ETOH (10 mL) is added K2CO3 (70 mg, 1.0 eq., 0.51 mmol) and the reaction is cooled to 0° C. with an ice bath. (1S)-Methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amine (82 mg, 1.0 equiv, 0.51 mmol) in 1.0 mL of EtOH is added via syringe in one portion and allowed to warm to ambient temperature over 3 h. Water (50 mL) and EtOAc (50 mL) is added and the EtOAc layer is washed with water (100 mL) and brine (50 mL) and dried over Na2SO4. Concentration and vacuum drying affords the title compound as a yellow gum. [mass expected (336.26); mass found (336.30)]

WORKUP

后处理

  1. temperatureto warm to ambient temperature over 3 h
  2. washthe EtOAc layer is washed with water (100 mL) and brine (50 mL)
  3. dry with materialdried over Na2SO4
  4. concentrationConcentration and vacuum
  5. customdrying