反応 #1446328
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04950702
反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Tripropylene glycol monomethyl ether (841.6 grams; 3.39 mol), benzoic acid (501.7 grams; 3.46 mol), zinc carbonate 13.5 grams) and toluene (100 ml) were placed into a two liter, three-necked round bottom flask equipped with stirrer, 10" Vigreux column, Dean Stark trap, condenser, heating mantle and thermometer. The reaction temperature was 173° .C at the beginning of the reaction and 235° C. after six hours and 48 minutes. During that time, water (70 ml) was removed. The reaction was continued the next day at 214° C. for an additional three hours and 45 minutes removing additional water (35 ml). Toluene was removed at 65° C. @ 45 mm Hg. The product was washed first with sodium carbonate (170 ml; 15%) at 95°-100° C. for 30 minutes, then with sodium carbonate (22 ml; 15%) and sodium hypochlorite (50 ml), then with sodium carbonate (22 ml; 15%) and sodium hypochlorite (25 ml) with water (300 ml) and finally a second time with water (300 ml). It was dried at 135° C. and filtered to give the desired product (1162.9 grams; 93.6% yield). The product assayed with the following properties: equipped with stirrer 10" Vigreux column, Dean Stark trap, condenser, heating mantle was 173° at the beginning of the reaction and 235° C. after six hours 48 minutes During that time, water (70 ml) was removed at 214° C. for an additional three hours 45 minutes removing additional water (35 ml) Toluene was removed at 65° C. @ 45 mm Hg The product was washed first with sodium carbonate (170 ml; 15%) at 95°-100° C. for 30 minutes It was dried at 135° C. filtered
ソース ID: ord-7eec73ed658a47418637831d1a8b4b7f