反应详情

温度

10 °C

To a solution of 2-methylheptan-2-ol (6.50 g.; 0.05 mole) in trifluoroacetic acid (20 ml) at -5° C. was added powdered methyleneaminoacetonitrile (3.40 g.; 0.05 mole) over 10 minutes. The slurry was allowed to warm to 10° C. and stirred until homogeneous (2 hours). After an additional 2 hours at 10° C., the reaction mixture was poured into water (100 ml) and the neutral material extracted with ether. The acid solution was basified with ammonia (pH 9-10) and the liberated base extracted into ether (3×80 ml). The combined extractswere dried over Na2SO4, filtered, and evaporated to dryness to give a colourless oil which was converted to the hydrogen fumarate salt, m.p. 156°-158° C.

1. waitAfter an additional 2 hours at 10° C.
2. extractionthe neutral material extracted with ether
3. extractionthe liberated base extracted into ether (3×80 ml)
4. dry with materialThe combined extractswere dried over Na2SO4
5. filtrationfiltered
6. customevaporated to dryness
7. customto give a colourless oil which