反应 #2320169

反应方程式

2-[(6-Methoxypyridin-3-ylamino)methylene]malonic acid diethyl ester

→

title compound

收率 73.1%

6-Methoxy-4-oxo-1,4-dihydro-[1,5]naphthyridine-3-carboxylic acid ethyl ester

收率 73.1%

溶剂

Dowtherm A

反应条件

后处理

1. 1
   其他(250° C.)
2. 2
   其他fitted with a still-head and a reflux condenser
3. 3
   温度The solution was heated
4. 4
   温度at reflux for an additional 15 min
5. 5
   其他to distil over
6. 6
   workup.ADDITIONdiluted with hexane (750 mL)
7. 7
   温度The mixture was cooled in ice for 1 h
8. 8
   过滤the brown solid was filtered off
9. 9
   洗涤washed with hexane
10. 10
    其他dried under vacuum

实验过程

Dowtherm A (Fluka, 500 mL) was brought to boiling (250° C.) in a 2 L 3-neck flask fitted with a still-head and a reflux condenser. 2-[(6-Methoxypyridin-3-ylamino)methylene]malonic acid diethyl ester (100 g, 0.34 mole) was added portion-wise over 5 min. The solution was heated at reflux for an additional 15 min, allowing some solvent to distil over. The resulting solution was cooled to room temperature and diluted with hexane (750 mL). The mixture was cooled in ice for 1 h, then the brown solid was filtered off, washed with hexane, and dried under vacuum to afford the title compound (61.72 g, 73%).

来源