反应详情

A solution of 3-phenoxybutan-2-one oxime (28.8 g.) in dry ether (150 ml.) was added dropwise, over 45 minutes, to a stirred, refluxing mixture of lithium aluminium hydride (6.3 g.) in dry ether (100 ml.). Stirring and heating were continued for 4 hours and the mixture was cooled and treated cautiously with water (6.3 ml.) followed by 15% aqueous sodium hydroxide (6.3 ml.), and finally, water (18.9 ml.). The mixture was stirred for 30 minutes and then filtered. The filtrate was extracted with 2N-hydrochloric acid (150 ml.) and the acid extract was made strongly basic with sodium hydroxide and extracted with ether. The ether extract was dried over anhydrous potassium carbonate, evaporated, and distilled to give a fraction, b.p. 118°-124°/14 mm. Redistillation gave pure 2-phenoxybut-3-ylamine, b.p. 116°-118°/14 mm.

1. temperaturerefluxing
2. temperatureheating
3. temperaturethe mixture was cooled
4. stirringThe mixture was stirred for 30 minutes
5. filtrationfiltered
6. extractionThe filtrate was extracted with 2N-hydrochloric acid (150 ml.)
7. extractionthe acid extract
8. extractionextracted with ether
9. extractionThe ether extract
10. dry with materialwas dried over anhydrous potassium carbonate
11. customevaporated
12. distillationdistilled
13. customto give a fraction, b.p. 118°-124°/14 mm
14. distillationRedistillation