HRID333093

反应详情

EQUATION

反应方程式

HRID 333093 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

6-Chloro-2-methylsulfanyl-pyrimidin-4-amine (176 mg, 1 mmol) was dissolved together with tert-butyl N-(2-aminoethyl)carbamate (200 mg, 1.25 mmol) and triethylamine (174 μl, 1.25 mmol) in THF (2 ml). The mixture was stirred at 180° C. under microwave heating for 8 hours. The mixture was diluted with ethyl acetate and the resulting solution was washed with a solution of sodium bicarbonate (5%) and brine, dried over magnesium sulfate, the volatiles were removed under reduced pressure. The residue dissolved in DCM and purified by filtration over silica to yield 105 mg (0.35 mmol, 35%) MS (ESI) m/z=300.2 [M+1]+.

WORKUP

后处理

  1. temperatureheating for 8 hours
  2. washthe resulting solution was washed with a solution of sodium bicarbonate (5%) and brine
  3. dry with materialdried over magnesium sulfate
  4. customthe volatiles were removed under reduced pressure
  5. dissolutionThe residue dissolved in DCM
  6. filtrationpurified by filtration over silica
  7. customto yield 105 mg (0.35 mmol, 35%)