反应详情

A solution of 4-azido-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (838 mg, 2.2 mmol), THF (10 ml) and P(Ph)3 (1.15 g, 4.4 mmol) and water (0.08 ml, 4.4 mmol) was refluxed for 6 hours and then concentrated in vacuo. The residue was dissolved in Et2O and treated with HCl (0.1N, 20 ml). The aqueous layer was extracted with Et2O, washed with Na2CO3 (10% aq.), dried over anhydrous MgSO4 and concentrated to afford the amine as colorless oil which was used in next step without further purification.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in Et2O
3. additiontreated with HCl (0.1N, 20 ml)
4. extractionThe aqueous layer was extracted with Et2O
5. washwashed with Na2CO3 (10% aq.)
6. dry with materialdried over anhydrous MgSO4
7. concentrationconcentrated