HRID903980

反应详情

EQUATION

反应方程式

HRID 903980 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

Into a mixture comprising 227 g of 5-amino-α-naphthol, 1 g of hydroquinone monomethyl ether and 2 liters of pyridine was dropwise added with stirring 110 g of methacrylic acid chloride cooled to -10° C. by the use of a coolant. After completion of the addition, the mixture was stirred at 0°-3° C. for 2 hours, followed by stirring at 25° C. for 2 hours. Thereafter, the reaction liquid was poured into 20 liters of water to form a precipitate which was then filtered, water-washed and then dried to obtain solids. The solids were added to 2 liters of a 1:1 mixture of methanol and a 5% sodium carbonate solution, and after stirring at 40° C. the mixture was poured into 4 liters of a 5% hydrochloric acid to form a large amount of precipitate. The precipitate was filtered by suction and then recrystallized from ethanol to obtain 210 g of N-(5-hydroxy-α-naphthyl)methacrylamide, m.p. 223°-224° C.

WORKUP

后处理

  1. additionAfter completion of the addition
  2. stirringby stirring at 25° C. for 2 hours
  3. customThereafter, the reaction liquid
  4. customto form a precipitate which
  5. filtrationwas then filtered
  6. washwater-washed
  7. customdried
  8. customto obtain solids
  9. customto form a large amount of precipitate
  10. filtrationThe precipitate was filtered by suction
  11. customrecrystallized from ethanol