反应详情

温度

70 °C

Glycine hydrochloride (400 g, 3.58 mol) was suspended in 8 L of n-butanol and thionyl chloride (1.37 L, 18.84 mol) was added slowly dropwise (exotherm). After addition was complete, the reaction was heated to 70° C. overnight. The reaction could be followed by spotting directly on TLC, pumping off the volatiles, eluting with 10% MeOH/CHCl3 saturated with NH3, and staining in ninhydrin. The next day the reaction was stripped to dryness under vacuum and the residue was triturated with heptane/EtOAc to give the product as a white solid after drying on a filter under Nitrogen.

1. additionAfter addition
2. customThe reaction
3. washeluting with 10% MeOH/CHCl3 saturated with NH3
4. customthe residue was triturated with heptane/EtOAc