反应详情

温度

80 °C

A sample of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-oxazepine-5(4H)-one hydrochloride, 16 g (0.058 mole), was dissolved in 65 ml of pyrrolidine. The stirred solution was heated to 80° C. for 3 hr. The solution was cooled to room temperature and dilute sodium hydroxide solution (50 ml) was added. The resulting solution was extracted with chloroform (3×30 ml) and concentrated in vacuo. The residue was taken up in boiling isopropyl alcohol (500 ml/ and fumaric acid (9.2 g, 0.079 mole) was added. The solution was filtered hot and the filtrate cooled to 20° C. for several hours. The resulting crystals, 14 g (47.8%) were collected and recrystallized from isopropyl alcohol, m.p. 147°-149° C.

1. temperatureThe solution was cooled to room temperature
2. extractionThe resulting solution was extracted with chloroform (3×30 ml)
3. concentrationconcentrated in vacuo
4. additionwas added
5. filtrationThe solution was filtered hot
6. temperaturethe filtrate cooled to 20° C. for several hours
7. customThe resulting crystals, 14 g (47.8%) were collected
8. customrecrystallized from isopropyl alcohol, m.p. 147°-149° C.