HRID1640111

反应详情

EQUATION

反应方程式

HRID 1640111 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

A suspension of methyl 7-methoxy-2-naphthoate (37.21 g, 172 mmol) in 48% aqueous HBr (195 mL, 1.72 mol) and AcOH (190 mL) was heated at 100° C. for 4 h. The mixture gradually went into solution and then precipitated. The reaction mixture was cooled to rt, and water was added. The solid was filtered and washed with water. The solid was dissolved in 1N NaOH and washed with Et2O. The aqueous solution was acidified to pH 1 with concentrated HCl. The precipitate was filtered and washed with water, then dried under vacuum to give 7-hydroxy-2-naphthoic acid as an off-white solid (32.3 g, 99%). LCMS: (FA) ES− 187.1.

WORKUP

后处理

  1. customprecipitated
  2. temperatureThe reaction mixture was cooled to rt
  3. additionwater was added
  4. filtrationThe solid was filtered
  5. washwashed with water
  6. dissolutionThe solid was dissolved in 1N NaOH
  7. washwashed with Et2O
  8. filtrationThe precipitate was filtered
  9. washwashed with water
  10. customdried under vacuum