反应详情

温度

-10 °C

27.6 g (97 mmoles) of Z-L-Phg-OH are dissolved in 300 ml of dry tetrahydrofuran, and 13.55 ml (97 mmoles) of triethylamine are added to the solution. The mixture is cooled to -10° C., and 12.1 ml (97 mmoles) of pivaloyl chloride are introduced. The suspension of the mixed anhydride is stirred for 10 minutes at -10° C., thereafter cooling is stopped and ammonia is bubbled through the suspension for one hour. Next day the reaction mixture is evaporated, and the residue is processed as described for the D enantiomer. 18.90 g (68.7%) of Z-L-Phg-NH2 are obtained; m.p.: 172°-173° C., Rf4 =0.75, [α]D =+80.7° (c=1.0, in dimethyl formamide).

1. temperaturecooling
2. customammonia is bubbled through the suspension for one hour
3. customNext day the reaction mixture is evaporated