反応 #50446

反応方程式

7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy] -3-hydroxy-phthalide

7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide

(ethoxycarbonylmethylene)-triphenyl-phosphorane

→

3-(ethoxycarbonylmethyl)-7[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   温度is maintained
2. 2
   その他The solvent is then evaporated off
3. 3
   その他the reaction material which remains is purified on a column of silica gel (eluant: ethyl acetate/n-hexane 1:1)

実験手順

A mixture of 1.5 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy] -3-hydroxy-phthalide (see Example 84) and 2.5 g of (ethoxycarbonylmethylene)-triphenyl-phosphorane is maintained at reflux temperature for 10 hours in approximately 40 ml of tetrahydrofuran. The solvent is then evaporated off and the reaction material which remains is purified on a column of silica gel (eluant: ethyl acetate/n-hexane 1:1) to yield 3-(ethoxycarbonylmethyl)-7[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide, m.p. 150°-152° C.

出典