HRID1731740

反应详情

EQUATION

反应方程式

HRID 1731740 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

55.2 g of sodium was added portionwise to 1500 ml of anhydrous methanol. When the reaction was complete 120 g of phenol and 200 g of 2-chloronicotinic acid were added, and the mixture was heated until completely solubilized. The methanol was removed by distillation, and the residue heated to 180°-200° C. for 5 minutes. The molten mass was cooled to about 100° C., and water was added slowly. The solution obtained was acidified with hydrochloric acid. After standing for about 16 hours, the solid obtained was filtered and dried, giving 237.4 g of 2-phenoxynicotinic acid, as white crystals, m.p. 179-181° C. (Kofler micro hot-stage); neutralization equivalent: 215.20 (calculated 216.55).

WORKUP

后处理

  1. additionwere added
  2. temperaturethe mixture was heated
  3. customThe methanol was removed by distillation
  4. temperaturethe residue heated to 180°-200° C. for 5 minutes
  5. additionwater was added slowly
  6. customThe solution obtained
  7. customthe solid obtained
  8. filtrationwas filtered
  9. customdried