反应详情

To a solution of diethyl 2-but-3-enyl-2-(tert-butoxycarbonylamino)propanedioate 81b (14.5 g, 4.4 mmol) in DCM (30 mL) was added TFA (10 mL), The mixture was stirred at room temperature for 16 h, quenched with saturated NaHCO3 (50 mL) and then extracted with DCM (150 mL) two times, washed with saturated NaHCO3 (100 mL) three times, dried over anhydrous sodium sulfate and concentrated in vacuo to afford diethyl 2-amino-2-but-3-enyl-propanedioate as a crude product (9.5 g, 94%), which was used for next step without further purification. MS: calc'd (MH+) 230, measured (MH+) 230.

1. customquenched with saturated NaHCO3 (50 mL)
2. extractionextracted with DCM (150 mL) two times
3. washwashed with saturated NaHCO3 (100 mL) three times
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo