HRID657074

反应详情

EQUATION

反应方程式

HRID 657074 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

6-({[4-(Methyloxy)phenyl]methyl}oxy)pyrido[2,3-b]pyrazin-3-yl trifluoromethanesulfonate (1.39 g, 3.35 mmol) was dissolved in dry toluene (100 mL) under argon and tetrabutylammonium bromide (2.16 g, 6.7 mmol) was added. The reaction was heated at 85° C. for 4 h; 1.08 g of tetrabutylammonium bromide were added and the reaction was heated at 90° C. for another 6 h; 0.54 g of bromide were added and the reaction was heated for 3 h. The reaction was cooled to rt, the toluene was evaporated, the residue was partitioned between water (200 mL) and diethyl ether (400 mL). The layers were separated and the aqueous was extracted with diethyl ether (2×300 mL). The organic phases were combined and washed with water (300 mL) then dried and evaporated to afford the title compound (1.19 g, 100%).

WORKUP

后处理

  1. temperaturethe reaction was heated at 90° C. for another 6 h
  2. temperaturethe reaction was heated for 3 h
  3. temperatureThe reaction was cooled to rt
  4. customthe toluene was evaporated
  5. customthe residue was partitioned between water (200 mL) and diethyl ether (400 mL)
  6. customThe layers were separated
  7. extractionthe aqueous was extracted with diethyl ether (2×300 mL)
  8. washwashed with water (300 mL)
  9. customthen dried
  10. customevaporated