HRID418047

反应详情

EQUATION

反应方程式

HRID 418047 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-phenylpyridine N-oxide (5 g) in DCM (50 ml) was added at RT TMSCN (4 ml), and the solution was stirred for 5 min at RT. Then, dimethylcarbamoyl chloride (2.8 ml) was added at RT, and the resulting solution was stirred at RT for 48 h. To the reaction mixture was added a solution of aq. 10% K2CO3 (50 ml) and stirring was continued for 10 min. The phases were separated and the aq. layer extracted twice with DCM. The combined org. phases were dried over MgSO4 and evaporated off. Filtration over a plug of SiO2 (Hept/EA 8:2) gave 4.98 g of the desired compound.

WORKUP

后处理

  1. stirringthe resulting solution was stirred at RT for 48 h
  2. stirringstirring
  3. waitwas continued for 10 min
  4. customThe phases were separated
  5. extractionthe aq. layer extracted twice with DCM
  6. dry with materialphases were dried over MgSO4
  7. customevaporated off
  8. filtrationFiltration over a plug of SiO2 (Hept/EA 8:2)