反应详情

温度

165 °C

A mixture of 18.8 g. (94 mmoles) of 1-(2-chloro-4-pyridyl)-1-ethylenedioxyethane and 50 ml. of ethylamine in 80 ml. of N-methyl-2-pyrrolidinone was sealed in a steel bomb and heated at 165° C. for 15 hours. The bomb was cooled and the contents distilled under reduced pressure to remove excess solvent. The residue in 100 ml. of methylene chloride was extracted with 2 N hydrochloric acid (3×25 ml.). The combined acid extracts were heated at 80° C. for 3 hours and were then cooled and made basic with sodium carbonate. The basified mixture was extracted with methylene chloride (4×25 ml.), and the combined organic extracts dried over sodium sulfate and evaporated to an oil which solidified, 11.5 g. (75%), m.p. 55°-57° C. The analytical sample was recrystallized from cyclohexane, m.p. 62°-63° C.

1. additionA mixture of 18.8 g
2. temperatureThe bomb was cooled
3. distillationthe contents distilled under reduced pressure
4. customto remove excess solvent
5. extractionof methylene chloride was extracted with 2 N hydrochloric acid (3×25 ml.)
6. temperatureThe combined acid extracts were heated at 80° C. for 3 hours
7. temperaturewere then cooled
8. extractionThe basified mixture was extracted with methylene chloride (4×25 ml.)
9. dry with materialthe combined organic extracts dried over sodium sulfate
10. customevaporated to an oil which
11. customThe analytical sample was recrystallized from cyclohexane, m.p. 62°-63° C.