hexyl 2-sulfanylacetate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Sodium antimonate obtained from U.S. Antimony Corporation (22.73 g, 0.0563 mole) was placed in the reaction vessel and the hexyl thioglycolate (100 ml, 0.5625 mole) added and stirred. Concentrated hydrochloric acid from Fisher Scientic Co. (9.52 ml, 0.1125 mole) was added dropwise, and an immediate temperature rise of 12° C. occurred. The mixture was thereafter heated and the byproduct of the reaction, water, was distilled over at 96° C. and collected. After 2 hours, a 92% yield of antimony (V) hexyl thioglycolate was obtained. The product was filtered to remove unreacted sodium antimonate and the additional byproduct of the reaction, sodium chloride. (9.52 ml, 0.1125 mole) was added dropwise an immediate temperature rise of 12° C. The mixture was thereafter heated was distilled over at 96° C. collected

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Thioglycolic acid obtained from Evans Chemetics, Inc. (75 ml, 1.0785 mole) was added dropwise to hexanol obtained from Continental Oil Company (135.6 ml, 1.0785 mole) with 12% Dowex cation exchange resin 50W×12 50/100 (12% cross-linking, 13.2 g) as a catalyst. The solution was stirred and a nitrogen atmosphere maintained. The mixture was thereafter heated, and the byproduct, water, was distilled over as an azeotrope with hexanol at 95° C. and collected. A 10 ml excess of hexanol was added to the reaction mixture to replace that lost in the azeotrope. After 2.5 hours, an 89% yield was obtained. A vacuum of 60 mm Hg was then applied to further the reaction without increasing the temperature. After an additional hour, a 95.9% yield of hexyl thioglycolate was obtained. a nitrogen atmosphere maintained The mixture was thereafter heated the byproduct, water, was distilled over as an azeotrope with hexanol at 95° C. collected A 10 ml excess of hexanol was added to the reaction mixture an 89% yield was obtained the reaction without increasing the temperature After an additional hour