反应 #1869222

反应方程式

methyl 6-bromo-1-ethyl-8-methyl-4-oxo-1,4-dihydroquinolone-3-carboxylate

2-amino-3-methylpyridine

XANTPHOS

cesium carbonate

→

Methyl 1-ethyl-8-methyl-6-(3-methylpyridin-2-ylamino)-4-oxo-1,4-dihydroquinolone-3-carboxylate

溶剂

acetonitrile

acetonitrile

dioxane

water

反应条件

后处理

1. 1
   workup.ADDITIONwere added
2. 2
   其他The pure product was isolated from the reaction solution by chromatography on an HPLC system
3. 3
   其他rose to 95% over the course of 20 minutes

实验过程

100 mg of methyl 6-bromo-1-ethyl-8-methyl-4-oxo-1,4-dihydroquinolone-3-carboxylate were transferred together with 40 mg of 2-amino-3-methylpyridine, 20 mg of Pd(OAc)2, 60 mg of XANTPHOS and 250 mg of cesium carbonate into a suitable reaction vessel, a protective gas atmosphere was generated with argon, and 10 ml of dioxane were added. The mixture was then heated at 80° C. for 8 h. The pure product was isolated from the reaction solution by chromatography on an HPLC system. This entailed use of a Merck Purospher RP-18 column and an acetonitrile:water mixture as eluent; the initial acetonitrile content was 15% and rose to 95% over the course of 20 minutes.

来源