反应详情

To a solution of 1.27 g of 1-hydroxy-2,4-dimethoxynaphthalene, prepared as shown in Preparations 7 and 8, in 50 ml of tetrahydrofuran was added 0.694 g of methyl chloroformate followed by 0.743 g of triethylamine. The mixture was stirred at room temperature for 16 hours, filtered, then the solvent removed under reduced pressure. The residue was dissolved in diethyl ether, washed with dilute hydrochloric acid and dried over anhydrous sodium sulfate. The ether was removed under reduced pressure and the residue chromatographed on silica gel, eluting with a 1:1 mixture of methylene chloride and hexane, to give 1-methoxycarbonyloxy-2,4-dimethoxynaphthalene, m.p. 128°-129° C.

1. filtrationfiltered
2. customthe solvent removed under reduced pressure
3. dissolutionThe residue was dissolved in diethyl ether
4. washwashed with dilute hydrochloric acid
5. dry with materialdried over anhydrous sodium sulfate
6. customThe ether was removed under reduced pressure
7. customthe residue chromatographed on silica gel
8. washeluting with a 1:1 mixture of methylene chloride and hexane