1-甲氧甲酰氨基-7-萘酚的合成

A Process for Preparation of 1-Methoxycarbonylamino-7-naphthol

在氮气保护下,添加≤0.6%抗结焦剂TA,1,7-克利夫酸与氢氧化钠和氢氧化钾混合碱,250℃反应5小时,得1-氨基-7-萘酚,纯度96.3%,收率88.9%后者以四氢呋喃为反应介质,与氯甲酸甲酯和碳酸氢钠20-25℃反应2小时,得到1-甲氧甲酰氨基-7-萘酚,灰黑色粉状结晶,熔点:105℃-107℃,纯度96.5%,收率76.4%。

1,7-Cleve's acid was heated with the mixture of sodium hydroxide and potassium hydroxide at 250℃ for 5 hours in the atmosphere of nitrogen and in the presence of =0.6% additive TA as the tar and coke retarding agent to give 1-amino-7-naphthol with the purity of 96.3% and yield of 88.9%. The product was reacted with methyl chloroformate at 20-25℃ for 2 hours in the presence of tetrahydrofuran and sodium bicarbonate to give 1-methoxycarbonylamino-7-naphthol a dark grey powder of melting point 105-107℃,with the purity of 96.5% and yield of 76.4%.