反应详情

To a stirring solution of 4-bromobenzoic acid-2,5-dioxo-pyrrolidin-1-yl ester (3.5 g, 11.7 mmol) [CAS: 80586-82-9] in tetrahydrofuran (0.15M), is added (S)-(+)-1-(2-pyrrolidinylmethyl)pyrrolidine (1.9 mL, 11.7 mmol) and the mixture heated to reflux for 4 h. The reaction is allowed to cool to room temperature and washed with water while extracting with 10% isopropanol/dichloromethane. The organic portion is dried with sodium sulfate, filtered; and concentrated in vacuo. The resulting residue is purified on a silica gel column, eluting with 2M ammonia in methanol and dichloromethane to obtain 2.80 g (71%) of the title compound. MS (ES+) m/e 337.1 (M+1)+.

1. temperaturethe mixture heated
2. temperatureto reflux for 4 h
3. washwashed with water
4. extractionwhile extracting with 10% isopropanol/dichloromethane
5. dry with materialThe organic portion is dried with sodium sulfate
6. filtrationfiltered
7. concentrationand concentrated in vacuo
8. customThe resulting residue is purified on a silica gel column
9. washeluting with 2M ammonia in methanol and dichloromethane