HRID485159

反应详情

EQUATION

反应方程式

HRID 485159 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl 5-(2-formyl-3-benzyloxyphenoxy)pentanoate (3.61 g, 0.01 M), potassium hydroxide (1.19 g, 0.021 M) and ethanol (40 ml) were stirred at 50°-60° C. for 5 hours. The ethanol was then removed in vacuo, the residue dissolved in water (50 ml) and the solution extracted with ether (2×80 ml). The aqueous layer was then acidified by the addition of 2N aqueous hydrochloric acid and the product extracted with ether (3×50 ml), and the combined extracts washed with water to neutrality, dried, and concentrated in vacuo to give 5-(2-formyl-3-benzyloxyphenoxy) pentanoic acid, 3.0 g, 91% as a yellow oil which crystallised on standing. The crude solid was crystallised from benzene/petroleum spirit 30°-40° C. to give pale cream crystals m.p. 110° C.

WORKUP

后处理

  1. customThe ethanol was then removed in vacuo
  2. dissolutionthe residue dissolved in water (50 ml)
  3. extractionthe solution extracted with ether (2×80 ml)
  4. additionThe aqueous layer was then acidified by the addition of 2N aqueous hydrochloric acid
  5. extractionthe product extracted with ether (3×50 ml)
  6. washthe combined extracts washed with water to neutrality
  7. customdried
  8. concentrationconcentrated in vacuo