反应详情

35 g (0.16 mol) of N-benzyl-2-pyrrolidone-3-carboxylic acid dissolved in 250 ml of absolute tetrahydrofuran is added dropwize, with stirring, to 12.2 g (0.32 mol) of lithium aluminium hydride in 350 ml of absolute tetrahydrofuran. After refluxing for 6 hours, 18.2 ml of water, 12.2 ml of 15% sodium hydroxide solution and 36.6 ml of water are added, whilst cooling with ice water. The precipitate formed is suction filtered and washed with tetrahydrofuran. The combined filtrates are concentrated by evaporation in vacuo and the residue obtained is purified over 900 g of aluminium oxide (neutral, activity II) with methylene chloride and then with increasing amounts of ethanol (up to 2%). Yield: 16 g (52.3% of theory), Rf value: 0.42 (aluminium oxide, neutral, eluant: 5% ethanol in methylene chloride).

1. additionis added dropwize
2. temperatureAfter refluxing for 6 hours
3. customThe precipitate formed
4. filtrationfiltered
5. washwashed with tetrahydrofuran
6. concentrationThe combined filtrates are concentrated by evaporation in vacuo
7. customthe residue obtained
8. customis purified over 900 g of aluminium oxide (neutral, activity II) with methylene chloride