反应详情

温度

5 °C

Freshly prepared nicotinoyl chloride hydrochloride (0.55 g, 0.003 mol) was suspended in methylene chloride (12 ml) cooled to 5° C. and sodium bicarbonate (0.053 g, 0.0063 mol) was added. After 5 minutes, desipramine hydrochloride (0.75 g, 0.0025 mol) was added and the mixture was stirred for 3 hours at 5° C. The sodium chloride was removed by filtration and the organic solution was extracted with aqueous sodium bicarbonate, dried over sodium sulfate, filtered through Celite™ and concentrated. Ethyl ether (5 ml) was added to the oily residue and white crystals formed. Yield 62% (0.58 g), m.p. 84°-86° C. The product has the formula: ##STR1616##

1. customThe sodium chloride was removed by filtration
2. extractionthe organic solution was extracted with aqueous sodium bicarbonate
3. dry with materialdried over sodium sulfate
4. filtrationfiltered through Celite™
5. concentrationconcentrated
6. additionEthyl ether (5 ml) was added to the oily residue and white crystals
7. customformed