反应详情

2.27 g of N,N′-carbonyldiimidazole (14 mmol, 1.4 eq) in a homogeneous suspension in 6 ml of ethyl acetate were added to 1.54 g of 2-amino-6-nitrophenol (10 mmol, 1 eq) in solution in 10 ml of ethyl acetate. The reaction medium was vigorously stirred for 3 hours, and then 10 ml of water were added. The stirring was continued for 15 minutes, before evaporating off approximately ¾ of the ethyl acetate. The reaction medium was brought to 0° C. and then 2 ml of 37% hydrochloric acid were added. The stirring was again continued for 15 minutes. The reaction medium was filtered. The solid obtained was washed with a 1 N hydrochloric acid solution, with water and with a water-ethanol (4:1) mixture, and then oven-dried. 1.3 g of product were obtained in the form of a pale yellow solid. Yield=73%.

1. waitThe stirring was continued for 15 minutes
2. custombefore evaporating off approximately ¾ of the ethyl acetate
3. customwas brought to 0° C.
4. addition2 ml of 37% hydrochloric acid were added
5. waitThe stirring was again continued for 15 minutes
6. filtrationThe reaction medium was filtered
7. customThe solid obtained
8. washwas washed with a 1 N hydrochloric acid solution, with water and with a water-ethanol (4:1) mixture
9. customoven-dried