2-chloro-N-(2-methylpropyl)acetamide

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: To a solution of triphenylphosphine (229.8 g, 876 mmol) in dry benzene (800 ml) was added N-isobutyl-2-chloroacetamide (131 g, 876 mmol) (prepared by standard methods from 2-chloroacetyl chloride and isobutylamine) in dry benzene (100 ml). The solution was heated under reflux, with vigorous stirring, for 8 hours. Upon cooling, colourless needles formed. These were collected by filtration and the filtrate heated under reflux for a further 8 hours. A second batch of the produce was collected. The combined batches were washed with dry ether and dried in vacuo to give 310 g (86% of theory) of N-isobutyl-acetamidotriphenyl-phosphonium chloride as colourless needles. The solution was heated under reflux, with vigorous stirring, for 8 hours Upon cooling colourless needles formed These were collected by filtration the filtrate heated under reflux for a further 8 hours A second batch of the produce was collected The combined batches were washed with dry ether dried in vacuo

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

実験手順: Chloroacetyl chloride (37.58 g) was added dropwise over 1 hour to a solution of isobutylamine (46.8 g) in ether (500 ml) maintaining the temperature below 5° C. Water (100 ml) was then added, and the organic layer was separated and washed with dilute hydrochloric acid, sodium hydroxide, and brine and dried (MgSO4). The solvent was removed in vacuo to yield N-isobutylchloroacetamide (47 g). maintaining the temperature below 5° C the organic layer was separated washed with dilute hydrochloric acid, sodium hydroxide, and brine dried (MgSO4) The solvent was removed in vacuo

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

実験手順: To a solution of triphenylphosphine (229.8 g, 876 mmol) in dry benzene (800 ml) was added N-isobutyl-2-chloroacetamide (131 g, 876 mmol) (prepared by standard methods from 2-chloroacetyl chloride and isobutylamine) in dry benzene (100 ml). The solution was heated under reflux, with vigorous stirring, for 8 hours. Upon cooling, colourless needles formed. These were collected by filtration and the filtrate heated under reflux for a further 8 hours. A second batch of the produce was collected. The combined batches were washed with dry ether and dried in vacuo to give 310 g (86% of theory) of N-isobutyl-acetamidotriphenyl-phosphonium chloride as colourless needles. The solution was heated under reflux, with vigorous stirring, for 8 hours Upon cooling colourless needles formed These were collected by filtration the filtrate heated under reflux for a further 8 hours A second batch of the produce was collected The combined batches were washed with dry ether dried in vacuo

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

実験手順: Chloroacetyl chloride (37.58 g) was added dropwise over 1 hour to a solution of isobutylamine (46.8 g) in ether (500 ml) maintaining the temperature below 5° C. Water (100 ml) was then added, and the organic layer was separated and washed with dilute hydrochloric acid, sodium hydroxide, and brine dried (MgSO4). The solvent was removed in vacuo to yield N-isobutylchloroacetamide (47 g). maintaining the temperature below 5° C the organic layer was separated washed with dilute hydrochloric acid, sodium hydroxide, and brine dried (MgSO4) The solvent was removed in vacuo

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

実験手順: Chloroacetyl chloride (ex. Aldrich) (50 g) was added dropwise, with stirring, to isobutylamine (ex. Aldrich) (70 ml) in dry ether (250 ml) at 0° C. When the mixture had reached room temperature it was worked up in conventional fashion to give N-isobutyl 2-chloroacetamide. The latter (20 g) was heated for 3 hours at 120° C. with triethylphosphite (23 g). The mixture was subjected to distillation in vacuo to give N-isobutyl diethylphosphono acetamide (22.5 g, bp. 140°-142.5° C. at 0.1 mm). had reached room temperature

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

実験手順: Chloroacetyl chloride (ex. Aldrich) (50 g) was added dropwise, with stirring to isobutylamine (ex. Aldrich) (70 ml) in dry ether (250 ml) at 0° C. When the mixture had reached room temperature it was worked up in conventional fashion to give N-isobutyl 2-chloroacetamide. The latter (20 g) was heated for 3 hours at 120° C. with triethylphosphite (23 g). The mixture was subjected to distillation in vacuo to give N-isobutyl diethylphosphono acetamide (22.5 g, bp. 140-142.5° C. at 0.1 mm). had reached room temperature