反应 #1310045
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US03933470
反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 4-amino-2-chlorophenol (21.45 grams, 0.15 mole) in dry DMF (150 ml.) and pyridine (11.8 grams) is added at 0°C. slowly dropwise with stirring isopropyl chloroformate (16.5 grams, 0.016 mole). After 4 hours at 0° C. to 5°C., a further one gram of isopropyl chloroformate is added. The mixture is stirred at 25°C. for 16 hours, then poured into ice-dilute hydrochloric acid. After 4 hours stirring and scratching, a solid separates out and is filtered off. Crystallization from methanol gives 14.5 grams, 42%, melting point 89°C. to 90°C. poured into ice-dilute hydrochloric acid After 4 hours stirring a solid separates out and is filtered off Crystallization from methanol gives 14.5 grams, 42%, melting point 89°C. to 90°C.
来源 ID: ord-98495b12889d46a7847e6e7f8b10d10e