反应详情

A mixed solution containing 46 g of 3-(p-aminobenzoyl)propionic acid hydrochloride, 25 g of 2-methyl-2-nitro-1-propanol, 1 g of benzyl triethyl ammonium chloride, 17 g of sodium hydroxide and 40 ml of water was heated under reflux for 6 hours. Then, 12 g of 2-methyl-2-nitro-1-propanol was added, and the mixture was further heated under reflux for 18 hours. Then 20% HCl was added. The solution was acidified (pH 2). The crystals which precipitated were collected by filtration. The crystals were washed with water and recrystallized from tetrahydrofuran to give 51.6 g of 3-[4-(2-methyl-2-nitropropylamino)benzoyl]propionic acid.

1. temperaturewas heated
2. temperatureunder reflux for 6 hours
3. temperaturethe mixture was further heated
4. temperatureunder reflux for 18 hours
5. customThe crystals which precipitated
6. filtrationwere collected by filtration
7. washThe crystals were washed with water
8. customrecrystallized from tetrahydrofuran