HRID1696748

反应详情

EQUATION

反应方程式

HRID 1696748 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 (0.100 g, 0.644 mmol), 1-iodo-2-fluoroethane, 0.123 g, 1.10 eq.), and 1.2 eq. of Cs2CO3 (0.252 g) in 1.0 mL of abs. acetonitrile, and the mixture allowed to react for 1 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=3/7) afforded 0.037 g of the title compound as brown solid.

WORKUP

后处理

  1. additionIn a glass vessel were mixed together the
  2. customto react for 1 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