反应详情

Methyl bromoacetate (16.8 g, 0.11 mol) was added, dropwise, to a stirred mixture of 2,5-dimethyl-3-pyrroline (10 g, 0.1 mol), potassium carbonate (13.8 g, 0.1 mol), and dimethylformamide (25 cm3) maintained below 30° C. by ice cooling. After addition was complete the mixture was cooled in ice for a further 1 h, then stirred at room temperature overnight. The reaction mixture was then diluted with water (50 cm3) and the product extracted into ether. The ether extract was dried and evaporated to yield an oil* which was distilled under vacuum to give methyl (trans-2,5-dihydro-2,5-dimethyl-1H-pyrrol-1-yl)acetate (7 g) b.p. 89°-92° C./15 mm.

1. temperaturemaintained below 30° C. by ice cooling
2. additionAfter addition
3. temperaturewas cooled in ice for a further 1 h
4. extractionthe product extracted into ether
5. extractionThe ether extract
6. customwas dried
7. customevaporated
8. customto yield an oil* which
9. distillationwas distilled under vacuum