反应详情

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.

1. temperatureThe solution was heated
2. temperatureunder reflux, with vigorous stirring, for 8 hours
3. temperatureUpon cooling
4. customcolourless needles formed
5. filtrationThese were collected by filtration
6. temperaturethe filtrate heated
7. temperatureunder reflux for a further 8 hours
8. customA second batch of the produce was collected
9. washThe combined batches were washed with dry ether
10. customdried in vacuo