反应详情

A solution of L-phenylglycine (10 g) in 40 mL of conc. sulfuric acid was cooled in an ice water/acetone bath. 90% Nitric acid (3.72 mL) was added dropwise over a 30 minute period at such a rate as to keep the internal temperature below 10° C. After addition was complete, stirring was continued for 1 hour at 0° C. and then the reaction mixture was allowed to warm to room temperature over 1.5 hours. The reaction mixture was poured onto 200 g of crushed ice and the resulting mixture was neutralized with sodium hydroxide to pH 7. The reaction mixture was diluted with 600 mL of water, Celite was added and the resulting suspension was filtered and concentrated to give the crude product D contaminated with sodium sulfate. This material was taken to the next step without further purification.

1. customthe internal temperature below 10° C
2. additionAfter addition
3. additionwas added
4. filtrationthe resulting suspension was filtered
5. concentrationconcentrated