6-methylheptyl 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:

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

実験手順: A mixture of 2.5 g of Amberlyst A-15, 71.0 g (0.763 mol) of thioglycolic acid and 109.8 g (0.843 mol) of 2-ethylhexanol is heated as described in Example 1, using a water separator, until no further water passes over. The residue is neutralized with 15 ml of a 10% sodium bicarbonate solution at 25° C. and washed with 15 ml of a 3% sodium chloride solution. After the aqueous phase (31.9 g of wash water polluted with thioglycolic acid) has been removed, the residue is distilled under reduced pressure (8.5 mbar) at an overhead temperature of 105° C. 129.5 g (82%) of the product are obtained with first runnings of 16.1 g and a residue of 4.9 g. is heated washed with 15 ml of a 3% sodium chloride solution After the aqueous phase (31.9 g of wash water polluted with thioglycolic acid) has been removed the residue is distilled under reduced pressure (8.5 mbar) at an overhead temperature of 105° C

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

実験手順: A mixture of 2.5 g of Amberlyst A-15, 71.0 g (0.763 mol) of thioglycolic acid and 109.8 g (0.843 mol) of 2-ethylhexanol is heated as described in Example 1, using a water separator, until no further water passes over. The residue is neutralized with 15 ml of a 10% sodium bicarbonate solution at 25° C. and washed with 15 ml of a 3% sodium chloride solution. After the aqueous phase (31.9 g of wash water polluted with thioglycolic acid) has been removed, the residue is distilled under reduced pressure (8.5 mbar) at an overhead temperature of 105° C. 129.5 g (82%) of the product are obtained with first runnings of 16.1 g and a residue of 4.9 g. is heated washed with 15 ml of a 3% sodium chloride solution After the aqueous phase (31.9 g of wash water polluted with thioglycolic acid) has been removed the residue is distilled under reduced pressure (8.5 mbar) at an overhead temperature of 105° C

反応条件: temp:12.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Sodium antimonate obtained from U.S. Antimony Corporation (19.2 g, 0.0476 mole) was placed in a reaction vessel and isooctyl thioglycolate from Evans Chemetics, Inc. (97.08 g, 0.4759 mole) added and stirred. Concentrated hydrochloric acid from Fisher Scientific Co. (9.5 ML, 0.0952 mole) was added dropwise and an immediate temperature increase of 12° C. was observed. The mixture was heated and the byproduct, water, was distilled over at 97° C. and collected. After 3.5 hours, a 93% yield of antimony (V) isooctyl thioglycolate was obtained. The resultant product was filtered to remove unreacted sodium antimonate and the additional byproduct of the reaction, sodium chloride. The product was then vacuum distilled at 3 mm Hg and a temperature range of 24°-100° C. to remove any unreacted isooctyl thioglycolate. (97.08 g, 0.4759 mole) added (9.5 ML, 0.0952 mole) was added dropwise The mixture was heated the byproduct, water, was distilled over at 97° C. collected

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

実験手順: A mixture of 2.5 g of Amberlyst A-15, 71.0 g (0.763 mol) of thioglycolic acid and 109.8 g (0.843 mol) of 2-ethylhexanol is heated as described in Example 1, using a water separator, until no further water passes over. The residue is neutralized with 15 ml of a 10% sodium bicarbonate solution at 25° C. and washed with 15 ml of a 3% sodium chloride solution. After the aqueous phase (31.9 g of wash water polluted with thioglycolic acid) has been removed, the residue is distilled under reduced pressure (8.5 mbar) at an overhead temperature of 105° C. 129.5 g (82%) of the product are obtained with first runnings of 16.1 g and a residue of 4.9 g. is heated washed with 15 ml of a 3% sodium chloride solution After the aqueous phase (31.9 g of wash water polluted with thioglycolic acid) has been removed the residue is distilled under reduced pressure (8.5 mbar) at an overhead temperature of 105° C