HRID1903425

反应详情

EQUATION

反应方程式

HRID 1903425 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In dimethylformamide (200 ml) are suspended 6-(22-hydroxydocosyl)-2,3-dimethoxy-5-methyl phenol (300 mg) and bis(4-hydroxysalicylidene)ethylenediiminocobalt(II) (50 mg). The suspension is stirred in an oxygen gas stream at ambient temperature and atmospheric pressure for 7 days. The insoluble matter is filtered off and the filtrate is concentrated under reduced pressure. The residue is diluted with water and extracted with ethyl acetate. The extract is treated in a conventional manner and the product is chromatographed on a silica gel column. The fractions obtained by elution with chloroform are pooled and recrystallized from ethanol to give orange-yellow needles of 6-(22-hydroxydocosyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (I, n=22). m.p. 89°-90.5° C.

WORKUP

后处理

  1. filtrationThe insoluble matter is filtered off
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. additionThe residue is diluted with water
  4. extractionextracted with ethyl acetate
  5. additionThe extract is treated in a conventional manner
  6. customthe product is chromatographed on a silica gel column
  7. customThe fractions obtained by elution with chloroform
  8. customrecrystallized from ethanol