2,2-dimethylpropane

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

実験手順: L-Gulonolactone is treated with acetone and dimethylpropane to give the lactone, 2,3:5,6-di-O-isopropylidene-L-gulonolactone.

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

実験手順: L-Gulonolactone is treated with acetone and dimethylpropane to give the lactone, 2,3:5,6-di-O-isopropylidene-L-gulonolactone.

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

実験手順: L-Gulonolactone is treated with acetone and dimethylpropane to give the lactone, 2,3:5,6-di-O-isopropylidene-L-gulonolactone.

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

実験手順: 4 g thiourea were dissolved in 20 ml ethanol at 60° C. The solution was then placed in a high pressure autoclave and subjected to a neopentane pressure of 150 bar. The solution was cooled down to room temperature within 60 h. The solution with h/g crystals was removed from the autoclave, filtered and the h/g crystals were washed with 10 ml cold ethanol. The h/g complex crystals were dried in the vacuum cabinet at 60° C. The solution with h/g crystals was removed from the autoclave filtered the h/g crystals were washed with 10 ml cold ethanol The h/g complex crystals were dried in the vacuum cabinet at 60° C.

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

実験手順: 4 g urea were dissolved in 12 ml ethanol at 60° C. The solution was then placed in a high pressure autoclave and subjected to a neopentane pressure of 150 bar. The solution was cooled down from 60° C. to room temperature within 48 h. The solution with h/g crystals was removed from the autoclave, filtered and the h/g crystals were washed with 10 ml cold ethanol. The h/g complex crystals were dried in the vacuum cabinet at 60° C. The solution was cooled down from 60° C. to room temperature within 48 h The solution with h/g crystals was removed from the autoclave filtered the h/g crystals were washed with 10 ml cold ethanol The h/g complex crystals were dried in the vacuum cabinet at 60° C.

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

実験手順: 4 g thiourea were dissolved in 20 ml ethanol at 60° C. The solution was then placed in a high pressure autoclave and subjected to a neopentane pressure of 150 bar. The solution was cooled down to room temperature within 60 h. The solution with h/g crystals was removed from the autoclave, filtered and the h/g crystals were washed with 10 ml cold ethanol. The h/g complex crystals were dried in the vacuum cabinet at 60° C. The solution with h/g crystals was removed from the autoclave filtered the h/g crystals were washed with 10 ml cold ethanol The h/g complex crystals were dried in the vacuum cabinet at 60° C.

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

実験手順: 4 g urea were dissolved in 12 ml ethanol at 60° C. The solution was then placed in a high pressure autoclave and subjected to a neopentane pressure of 150 bar. The solution was cooled down from 60° C. to room temperature within 48 h. The solution with h/g crystals was removed from the autoclave, filtered and the h/g crystals were washed with 10 ml cold ethanol. The h/g complex crystals were dried in the vacuum cabinet at 60° C. The solution was cooled down from 60° C. to room temperature within 48 h The solution with h/g crystals was removed from the autoclave filtered the h/g crystals were washed with 10 ml cold ethanol The h/g complex crystals were dried in the vacuum cabinet at 60° C.

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

実験手順: A solution of 2,2-Dimethylpropane (15.1 g, 0.10 mol) in dry tetrahydrofuran (80 ml) was added dropwise to a mixture of magnesium turnings (2.43 g, 0.10 mol) in dry tetrahydrofuran (20 ml) containing a single crystal of iodine, at such a rate so as to maintain the solvent at reflux. The resulting solution was allowed to cool to room temperature and decanted from the residual magnesium under nitrogen into a fresh flask. The solution was diluted with dry tetrahydrofuran (150 ml), cooled to -20° C. under an atmosphere of nitrogen treated with cuprous bromide dimethyl sulphide complex and stirred for 20 minutes. The resulting solution was then treated with 4-bromo-1-butene (13.5 g, 0.10 mol) and stirred at -20° C. for 16 hours and then at 20° C. for 4 hours. The reaction mixture as quenched with saturated aqueous ammonium chloride solution (10 ml), diluted with ether (200 ml) and washed with an aqueous solution of ammonia (2×200 ml of 10%). The solution was dried over sodium sulfate and distilled at atmospheric pressure to yield 6,6-dimethyl- 1-heptene as a colourless oil, having a boiling point of 120°-125° C., and the following structural characteristics: at such a rate so as to maintain the solvent at reflux decanted from the residual magnesium under nitrogen into a fresh flask The solution was diluted with dry tetrahydrofuran (150 ml) cooled to -20° C. under an atmosphere of nitrogen treated with cuprous bromide dimethyl sulphide complex stirred at -20° C. for 16 hours at 20° C. for 4 hours The reaction mixture as quenched with saturated aqueous ammonium chloride solution (10 ml) diluted with ether (200 ml) washed with an aqueous solution of ammonia (2×200 ml of 10%) The solution was dried over sodium sulfate distilled at atmospheric pressure

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

実験手順: L-Gulonolactone is treated with acetone and dimethylpropane to give the lactone, 2,3:5,6-di-O-isopropylidene-L-gulonolactone.

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

実験手順: 4 g thiourea were dissolved in 20 ml ethanol at 60° C. The solution was then placed in a high pressure autoclave and subjected to a neopentane pressure of 150 bar. The solution was cooled down to room temperature within 60 h. The solution with h/g crystals was removed from the autoclave, filtered and the h/g crystals were washed with 10 ml cold ethanol. The h/g complex crystals were dried in the vacuum cabinet at 60° C. The solution with h/g crystals was removed from the autoclave filtered the h/g crystals were washed with 10 ml cold ethanol The h/g complex crystals were dried in the vacuum cabinet at 60° C.

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

実験手順: 4 g urea were dissolved in 12 ml ethanol at 60° C. The solution was then placed in a high pressure autoclave and subjected to a neopentane pressure of 150 bar. The solution was cooled down from 60° C. to room temperature within 48 h. The solution with h/g crystals was removed from the autoclave, filtered and the h/g crystals were washed with 10 ml cold ethanol. The h/g complex crystals were dried in the vacuum cabinet at 60° C. The solution was cooled down from 60° C. to room temperature within 48 h The solution with h/g crystals was removed from the autoclave filtered the h/g crystals were washed with 10 ml cold ethanol The h/g complex crystals were dried in the vacuum cabinet at 60° C.