反应详情

A mixture of 6-methoxycarbonyl-1-carboxy-3-hexyne [VI-1] (18.4 g, 0.1 mole), furan (13.6 g, 0.2 mole), dichloroacetic anhydride (28.8 g, 0.12 mole), boron trifluoride ether complex (3.2 g) and toluene (100 ml) is reacted at 20°-30° C. for 10 hours. After completion of the reaction, the reaction mixture is cooled, and washed successively with water, 5% aqueous sodium carbonate solution and water, and the organic layer is dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography to give 1-oxo-1-furyl-7-methoxycarbonyl-4-heptyne [VII-1] (15.2 g, yield; 65%), b.p. 120°-125° C./0.3 mmHg.

1. customis reacted at 20°-30° C. for 10 hours
2. customAfter completion of the reaction
3. temperaturethe reaction mixture is cooled
4. washwashed successively with water, 5% aqueous sodium carbonate solution and water
5. dry with materialthe organic layer is dried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe resulting residue is purified by silica gel column chromatography