反应详情

Sodium hydride (60% in oil) (10 mg, 0.25 mmol) was added to a solution of 3-Formylamino-pyrrolidine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl ester (2T) (50 mg, 0.183 mmol) in THF (3 ml). DMF (1 ml) was added and stirred for 1 hour. Methyl iodide (0.1 ml, 1.60 mmol) was added and the reaction was stirred overnight. The solvent was evaporated and the residue extracted with EtOAc (50 ml), washed with H2O (20 ml), dried over MgSO4, filtered and solvent evaporated yielding a residue which chromatographed on silica gel eluting with 3% MeOH/MeCl2 yielding 3T (50 mg, 94%). LCMS (MH 287) Retention time=2.77 minutes.

1. stirringthe reaction was stirred overnight
2. customThe solvent was evaporated
3. extractionthe residue extracted with EtOAc (50 ml)
4. washwashed with H2O (20 ml)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customsolvent evaporated
8. customyielding a residue which
9. customchromatographed on silica gel eluting with 3% MeOH/MeCl2 yielding 3T (50 mg, 94%)