反应详情

To a solution of N2-(tert-butoxycarbonyl)-N2-methyl-N-[3-(triphenylphosphonio)propyl]glycinamide chloride (7.6 g, 14 mol) in methylene chloride (38 mL) and methanol (4.2 mL) was added 2.0 M HCl in diethyl ether (16 mL, 32 mmol), and the mixture was stirred overnight at room temperature. The solution was cooled to 0° C. and treated with 7 M ammonia in methanol (6.0 mL, 42 mmol), giving an immediate white precipitate. After 30 minutes, the slurry was filtered and the flask and filter cake were rinsed with methylene chloride (68 mL). The filtrate was concentrated to give the title compound (6.2 g, 100%) as a crude white solid.

1. temperatureThe solution was cooled to 0° C.
2. customgiving an immediate white precipitate
3. waitAfter 30 minutes
4. filtrationthe slurry was filtered
5. filtrationthe flask and filter cake
6. washwere rinsed with methylene chloride (68 mL)
7. concentrationThe filtrate was concentrated