反応 #71010

反応方程式

(9-oxo-9H-thioxanthen-2-yloxy)acetic acid

acetonitrile

4-hydroxybutylacrylate glycidylether

→

yellow oil

収率 144.2%

acrylic acid 4-{2-hydroxy-3-[2-(9-oxo-9H-thioxanthen-2-yloxy)-acetoxy]-propoxy}-butyl ester

収率 144.2%

溶媒

dimethylacetamide

反応条件

後処理

1. 1
   温度was heated to reflux
2. 2
   温度at reflux temperature for 16 hours
3. 3
   その他the solvent was evaporated under reduced pressure

実験手順

A reaction mixture containing (9-oxo-9H-thioxanthen-2-yloxy)acetic acid (4.0 g, 14 mmol), acetonitrile (55 ml), dimethylacetamide (10 mL), tetrabutylammonium bromide (0.5 g, 1.4 mmol) and 2,6-di-tert-butyl-4-methylphenol (0.03 g, 0.114 mmol) was heated to reflux. At this temperature 4-hydroxybutylacrylate glycidylether (2.3 g, 11.4 mmol) was added and the mixture was allowed to stir at reflux temperature for 16 hours. The mixture was cooled to room temperature and the solvent was evaporated under reduced pressure to provide 8.0 g of a yellow oil. The product was purified on a Prochrom LC80 Column using Kromasil Si 60A 10 μm as silica and dichloromethane/ethyl acetate (60/40) as eluent, to afford 1.8 g of a yellow oil.

出典