反应详情

温度

100 °C

10.2 g 4-(p-fluorobenzoyl)-piperidine and 16.5 g 7-(chloropropyl)-theophylline are carefully mixed in the solid state and heated to 100° C. in a round flask in an oil bath. The mixture at first results in a clear melt, subsequently begins to crystallize and then changes into a solid mass. It is allowed to cool after 10 minutes, dissolved in ethyl acetate and 2n hydrochloric acid is added, whereby a dark oil separates in the organic phase, crystallizing on standing overnight. By recrystallizaing with 100 ml carbon tetrachloride, an intially oily then crystallizing substance is obtained, 7.4 g of the product with an mp of 114° to 119° C. (yield: 43.5%)

1. customThe mixture at first results in a clear melt
2. customto crystallize
3. temperatureto cool after 10 minutes
4. dissolutiondissolved in ethyl acetate
5. addition2n hydrochloric acid is added
6. customwhereby a dark oil separates in the organic phase, crystallizing
7. customan intially oily then crystallizing substance
8. customis obtained