反应详情

2.4 g of N-[2-(7-methoxy-1,4-dihydro-indeno[1,2-b]pyrrol-1-yl)-ethyl]-acetamide were heated to 140° for 17 hours under argon in 48 ml of ethylene glycol/water 2:1 in the presence of 2.5 g of potassium hydroxide. The mixture was left to cool and treated with 250 ml of semi-saturated sodium chloride solution. The mixture was extracted three times with diethyl ether and the combined extracts were dried over sodium sulfate, filtered and evaporated. The brown oil was dissolved in 30 ml of methanol and treated with 1.0 g of fumaric acid, following which pale brown crystals separated. These were dissolved in 120 ml of warm methanol. After cooling to room temperature the product was crystallized out by the slow addition of 120 ml of diethyl ether. 2.0 g (66%) of 2-(7-methoxy-1,4-dihydro-indeno[1,2-b]pyrrol-1-yl)-ethylamine fumarate (1:1) with m.p. 177°-180° were obtained.

1. waitThe mixture was left
2. temperatureto cool
3. extractionThe mixture was extracted three times with diethyl ether
4. dry with materialthe combined extracts were dried over sodium sulfate
5. filtrationfiltered
6. customevaporated
7. dissolutionThe brown oil was dissolved in 30 ml of methanol
8. additiontreated with 1.0 g of fumaric acid
9. customseparated
10. dissolutionThese were dissolved in 120 ml of warm methanol
11. customwas crystallized out by the slow addition of 120 ml of diethyl ether