反应详情

19 cm3 of ethyl ketomalonate and 2.5 cm3 of pyridine were added to 23.1 g of 4-benzyloxyacetophenone. The reaction medium was heated and maintained at reflux for 12 hours. After cooling, the reaction medium was purified by chromatography on silica gel (particle size 40-63 μm, under an argon pressure of 150 kPa), eluting with a mixture of dichloromethane and methanol (99/1 by volume). The fractions containing the product were combined and then concentrated under reduced pressure (45° C.; 5 kPa). The product obtained was triturated in 150 cm3 of ethanol, filtered through a sinter funnel, washed with twice 50 cm3 of ethanol and 50 cm3 of isopropyl ether to give, after drying under reduced pressure (2 kPa; 55° C.), 5.6 g of diethyl hydroxy[2-(4-benzyloxyphenyl)-2-oxoethyl]malonate melting at 80° C.

1. temperatureThe reaction medium was heated
2. temperaturemaintained
3. temperatureat reflux for 12 hours
4. temperatureAfter cooling
5. customthe reaction medium was purified by chromatography on silica gel (particle size 40-63 μm
6. washunder an argon pressure of 150 kPa), eluting with a mixture of dichloromethane and methanol (99/1 by volume)
7. additionThe fractions containing the product
8. concentrationconcentrated under reduced pressure (45° C.; 5 kPa)
9. customThe product obtained
10. customwas triturated in 150 cm3 of ethanol
11. filtrationfiltered through a sinter funnel
12. washwashed with twice 50 cm3 of ethanol and 50 cm3 of isopropyl ether
13. customto give
14. dry with materialafter drying under reduced pressure (2 kPa; 55° C.), 5.6 g of diethyl hydroxy[2-(4-benzyloxyphenyl)-2-oxoethyl]malonate melting at 80° C.