HRID2112819

反应详情

EQUATION

反应方程式

HRID 2112819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.24 mL (2.0 mmol) of 4-methylpiperidine and 0.28 mL (2.0 mmol) of triethylamine are added to a solution of 0.51 g (2.0 mmol) of 6-bromo-2-chloro-4-methylquinoline in 15 mL of 1,4-dioxane and the reaction mixture is refluxed overnight. After cooling, the precipitate is filtered off, the filtrate is evaporated down, the residue is combined with acetonitrile and MTBE, filtered to remove insoluble ingredients, and the filtrate is evaporated down again. Yield: 0.69 g (100% of theoretical); C16H19BrN2 (M=319.240); calc.: molpeak (M+H)+: 319/321 (Br); found: molpeak (M+H)+: 319/321 (Br); HPLC-MS: 4.7 min (method B).

WORKUP

后处理

  1. temperaturethe reaction mixture is refluxed overnight
  2. temperatureAfter cooling
  3. filtrationthe precipitate is filtered off
  4. customthe filtrate is evaporated down
  5. filtrationfiltered
  6. customto remove insoluble ingredients
  7. customthe filtrate is evaporated down again
  8. custom4.7 min (method B)