反应详情

(+)-α-Chloro-2-aminobenzenepropanoic acid 2,6-dimethylpiperidine salt (1.25 g., 4.00 mmol) was added to magnetically stirred N sodium hydroxide (4 ml.) under nitrogen. The solution was stirred under nitrogen overnight at room temperature. The pH was adjusted to a value between 2 and 3 (pH paper) with conc. hydrochloric acid while cooling in ice. The crystalline precipitate was collected and washed with several aliquots of ice cold water. The product was dried briefly under vacuum over phosphorus pentoxide and then stirred with ether. The product was dried over phosphorus pentoxide at 56° C. for several hours under oil pump vacuum to give 0.48 g. (74%) of the title compound, m.p. 155°-157° C., [α]D25 +36.09° (c 0.87, DMF).

1. temperaturewhile cooling in ice
2. customThe crystalline precipitate was collected
3. washwashed with several aliquots of ice cold water
4. dry with materialThe product was dried briefly under vacuum over phosphorus pentoxide
5. stirringstirred with ether
6. dry with materialThe product was dried over phosphorus pentoxide at 56° C. for several hours under oil pump vacuum
7. customto give 0.48 g