反应 #3123584
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04411902
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 52 ml of 2,5-dimethoxy-tetrahydrofuran (0.402 moles) are dissolved in 58 ml of water and acidified with 1.2 ml of 37% hydrochloric acid. After 15 minutes, 58 g of acetonedicarboxylic acid (0.397 moles) are added followed by 40.4 g of tribasic sodium citrate bihydrate (0.137 moles) dissolved in 58 ml of water. 18.5 g of ethylamine (0.411 moles) in 35 ml of water are then dripped in. The mixture is left stirring until carbon dioxide ceases to be evolved. It is then saturated with K2CO3 and extracted with ethyl ether. After drying and evaporating the solvent, the crude product is distilled under vacuum. 27.9 g of 8-ethyl-8-azabicyclo-[3.2.1]-octan-3-one are obtained. The mixture is left saturated with K2CO3 and extracted with ethyl ether After drying evaporating the solvent the crude product is distilled under vacuum
来源 ID: ord-d7fc5ef1874843058f1260b1529652ea