HRID1696751

反应详情

EQUATION

反应方程式

HRID 1696751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a glass vessel were mixed together the above prepared 4-methylsulfanyl-pyridine-2,6-diamine (0.350 g, 2.25 mmol), tert-butyl-(2-iodo-ethoxy)-dimethyl-silane (CAS 101166-65-8, 0.700 g, 1.08 eq.), and 1.2 eq. of Cs2CO3 (0.882 g) in 3.5 mL of abs. acetonitrile, and the mixture allowed to react for 2 h at 125° C. in a microwave oven. Cooling, pouring onto crashed ice, twofold extraction with AcOEt, washing with water and brine, drying over sodium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, hexane/AcOEt=4/6) afforded 0.155 g of the title compound as light brown oil.

WORKUP

后处理

  1. additionIn a glass vessel were mixed together the
  2. customto react for 2 h at 125° C. in a microwave oven
  3. temperatureCooling
  4. additionpouring
  5. extractionice, twofold extraction with AcOEt
  6. washwashing with water and brine
  7. dry with materialdrying over sodium sulfate, and evaporation of the solvents