反应详情

Trans-1-(p-Nitrobenzyloxycarbonyl)-4-hydroxy-L-proline p-methoxybenzyl ester (49 g) was dissolved in 300 ml of dry tetrahydrofuran, and 33 ml of triethylamine, 9.59 g of 4-dimethylaminopyridine and 33.2 g of benzoyl chloride were added thereto, followed by stirring under reflux for 5 hours. The reaction mixture was cooled down to room temperature and distilled to remove the solvent. The residue was diluted with ethyl acetate, washed successively with water, dilute hydrochloric acid, water, a saturated sodium bicarbonate solution and water, dried over anhydrous sodium sulfate and distilled to remove the solvent. Recrystallization of the residue from diethyl ether gave trans-1-(p-nitrobenzyloxycarbonyl)-4-benzoyloxy-L-proline p-methoxybenzyl ester.

1. temperatureunder reflux for 5 hours
2. distillationdistilled
3. customto remove the solvent
4. additionThe residue was diluted with ethyl acetate
5. washwashed successively with water, dilute hydrochloric acid, water
6. dry with materiala saturated sodium bicarbonate solution and water, dried over anhydrous sodium sulfate
7. distillationdistilled
8. customto remove the solvent
9. customRecrystallization of the residue from diethyl ether