反应 #3733560
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06605124B1
反应条件: temp:15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 2 ml of chloroacetyl chloride (25.4 mmol) were added dropwise to a suspension of 5 g of 2-amino-1-naphthol hydrochloride (25.4 mmol) and 5.08 g of calcium carbonate in 200 ml of dioxane, with stirring and under an inert atmosphere. The reaction medium was stirred at 40° C. for 1 hour 30 minutes, cooled to 15° C., filtered on sintered glass and the inorganic salts were rinsed twice with ethyl acetate. The combined organic phases were concentrated until an insoluble product appeared. The concentrate was poured over 250 ml of ice-cold water. The precipitate formed was drained, washed with water and dried under vacuum to a constant weight to give 3.58 g of 2-chloro-N-(1-hydroxynaphthalen-2-yl)acetamide in the form of a beige powder with a yield of 60%. The reaction medium was stirred at 40° C. for 1 hour 30 minutes filtered on sintered glass the inorganic salts were rinsed twice with ethyl acetate The combined organic phases were concentrated until an insoluble product The concentrate was poured over 250 ml of ice-cold water The precipitate formed washed with water dried under vacuum to a constant weight
来源 ID: ord-a4523548cc834107a28ffc52c65cc4cd