反应详情

To a mixture of 2-(6-Hydroxy-naphthalen-2-yl)-propionic acid methyl ester 6 (150 g, 652 mmol), anhydrous K2CO3 (480 gr, 3.473 mol) and sodium iodide (22.5 grams, 150 mmol) in anhydrous acetone (2000 ml) was added methyl 6-bromohexanoate (216 g, 1.033 mol) and refluxed for 60 hours. Acetone was distilled off and water (1500 ml) was added. Crude 9 was extracted into ethyl acetate, dried over Na2SO4, distilled and purified by column chromatography on silica gel using hexane as eluant to give pure 2 (130 g, 55.6%) as a light yellow syrup. The structure was confirmed with NMR.

1. temperaturerefluxed for 60 hours
2. distillationAcetone was distilled off
3. additionwater (1500 ml) was added
4. extractionCrude 9 was extracted into ethyl acetate
5. dry with materialdried over Na2SO4
6. distillationdistilled
7. custompurified by column chromatography on silica gel