反应 #2824862
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04009187
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 6.13 g of phosphorous oxychloride were added, while stirring, to 2.93 g of dimethyl formamide at 5°-10° C for 5 minutes. The mixture was kept at 0°-5° C for 40 minutes and then heated to room temperature. Immediately, and with vigorous stirring, 8.96 g of 8-(2-furyl)-octanoic acid methyl ester were added, whereupon the mixture was cooled to 5°-10° C in an ice-salt bath during 1 hour. After further 1 hour at room temperature, 40 g of ice were added, whereupon the mixture was neutralized with 10 g of sodium carbonate. The two phases were then separated, and the aqueous phase was extracted with ether. The combined organic phases were dried and then distilled. Boiling point 144° C at 0.2 mm Hg. was cooled to 5°-10° C in an ice-salt bath during 1 hour After further 1 hour at room temperature The two phases were then separated the aqueous phase was extracted with ether The combined organic phases were dried distilled
来源 ID: ord-16aa0f062e594790be7dc431eeea9cad