HRID1381087

反应详情

EQUATION

反应方程式

HRID 1381087 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

12.3 g of 1,4-dihydroxy-2-naphthoic acid was dissolved in 100 ml of dimethylformamide, and to the solution was added 23.2 g of a 28% methanolic solution of sodium methylate in a nitrogenous atmosphere at 40° C. with stirring. The mixture was heated to 60° C., and 15.3 g of hexadecyl bromide was added thereto dropwise over a period of 30 minutes. The resulting mixture was heated for 3 hours while stirring, cooled, and then poured into 1 liter of ice-water to which 50 ml of concentrated hydrochloric acid had already been added with stirring. The precipitated crude crystals were filtered and washed with water. After addition of 1 g of activated carbon, the mixture was dissolved in 100 ml of methanol while heating. The activated carbon was filtered, and the filtrate was cooled. The precipitated crystals were filtered, washed with methanol and dried to obtain 9.4 g of 1-hydroxy-4-hexadecyloxy-2-naphthoic acid. Melting Point: 121°-124° C.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated for 3 hours
  2. stirringwhile stirring
  3. temperaturecooled
  4. additionhad already been added
  5. stirringwith stirring
  6. customThe precipitated crude crystals
  7. filtrationwere filtered
  8. washwashed with water
  9. additionAfter addition of 1 g of activated carbon
  10. dissolutionthe mixture was dissolved in 100 ml of methanol
  11. temperaturewhile heating
  12. filtrationThe activated carbon was filtered
  13. temperaturethe filtrate was cooled
  14. filtrationThe precipitated crystals were filtered
  15. washwashed with methanol
  16. customdried