HRID2412846

反应详情

EQUATION

反应方程式

HRID 2412846 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 15 ml of methanol is dissolved 300 mg of methyl 22-(2-hydroxy-3,4-dimethoxy-6-methylphenyl)docosanoate followed by addition of 20 ml of a 14% aqueous solution of sodium hydroxide. The mixture is stirred at 50°-60° C. for 1.5 hours. The reaction mixture is made acidic with 3N--HCl and extracted with ethyl acetate. The extract is washed with water and, after drying, the solvent is distilled off under reduced pressure. The residue is recrystallized from methanol to obtain 22-(2-hydroxy-3,4-dimethoxy-6-methylphenyl)docosanoic acid (IV:n=21), m.p. 67° C.-68° C. NMR(δ, in deuteriochloroform): 1.27(38H,b,CH2), 2.24(3H,s,nuclear CH3), 2.28-2.56(4H,m,CH2COO, nuclear CH2), 3.80(3H,s,OCH3), 3.84(3H,s,OCH3), 6.24(1H,s, nuclear H)

WORKUP

后处理

  1. extractionHCl and extracted with ethyl acetate
  2. washThe extract is washed with water
  3. customafter drying
  4. distillationthe solvent is distilled off under reduced pressure
  5. customThe residue is recrystallized from methanol