反应 #1595787
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04066635
反应条件: temp:-20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 111.7 g of benzyloxycarbonyl-β-alanine were dissolved in 1 liter of dimethylformamide, cooled to -20° C, treated with 70 ml of triethylamine and 67 ml of chloroformic acid isobutyl ester and stirred at -20° C for 3 minutes. Dry ammonia gas was led into this mixture until the pH rose to 11, care being taken that the temperature did not, exceed -10° C. The mixture was stirred for a further 30 minutes at room temperature, filtered and the filtrate concentrated in vacuo. The residue was recrystallised from water. Yield: 91 g; melting point 162°-165° C. exceed -10° C The mixture was stirred for a further 30 minutes at room temperature filtered the filtrate concentrated in vacuo The residue was recrystallised from water
来源 ID: ord-b937ca86ce254ef1a0c438fd8ef55554