反应详情

The polar diastereoisomer of 3-(1H-indol-3-yl)pyrrolidine-1-carboxylic acid-(4-dimethylamino-4-phenylcyclohexyl-methyl)-amide (115 mg, 0.241 mmole) was dissolved in abs. ethanol (1.5 ml). Citric acid (46.8 mg, 0.244 mmole) was added in one portion at ca. 40° C. while stirring. No precipitate formed at RT. The amount of solvent was reduced to 2 ml in vacuo and diethyl ether (20 ml) was then added. After stirring overnight at RT the precipitate was filtered off, washed with diethyl ether (3×3 ml) and dried in vacuo. The non-polar diastereoisomer of 3-(1H-indol-3-yl)pyrrolidine-1-carboxylic acid-(4-dimethylamino-4-phenylcyclohexylmethyl)-amide citrate (312 mg, 94%, Example 52) was a pale beige solid.

1. customNo precipitate formed at RT
2. additionwas then added
3. stirringAfter stirring overnight at RT the precipitate
4. filtrationwas filtered off
5. washwashed with diethyl ether (3×3 ml)
6. customdried in vacuo