반응 #50445

반응 방정식

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

triethylamine

hydrochloric acid

acetyl chloride

→

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

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate
2. 2
   세척the organic phase is washed with sodium chloride solution
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   농축concentrated by evaporation under reduced pressure

실험 절차

1.3 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide (see Example 84) are dissolved in 10 ml of tetrahydrofuran, and 0.6 ml of triethylamine is added to the solution which is then treated dropwise at 25° C. (internal temperature) with 0.5 ml of acetyl chloride. After subsequently stirring for 2 hours at room temperature, the reaction mixture is treated with ice-water and dilute hydrochloric acid and extracted with ethyl acetate, and the organic phase is washed with sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure. Column chromatography on silica gel [eluant: ethyl acetate/n-hexane (2:3)] yields 3-acetoxy-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide in the form of white crystals, m.p. 119°-120° C.

출처