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HRID2231467

反应详情

EQUATION

反应方程式

HRID 2231467 的结构方程式

REACTANTS

反应物

3
结构：O=C([O-])[O-].[K+].[K+]
HCID11430

Potassium Carbonate

CK2O3

2 次

结构：CS(=O)(=O)OCCOCCOS(C)(=O)=O
HCID147571

Ethanol, 2,2'-oxybis-, dimethanesulfonate

C6H14O7S2

结构：CCCc1c(OCCCC(=O)OCC)ccc(C(C)=O)c1O
HCID14330004

Ethyl 4-(4-acetyl-3-hydroxy-2-propylphenoxy)butanoate

C17H24O5

PRODUCTS

生成物

1
结构：CCCc1c(OCCCC(=O)OCC)ccc(C(C)=O)c1OCCOCCOS(C)(=O)=O
HCID14330009

未命名化合物

收率 67%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CC(C)=O
溶剂HCID180

Acetone

C3H6O

结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

PROCEDURE

实验过程

A mixture of 4 g (0.013 mol) of 4-(4-acetyl-3-hydroxy-2-propylphenoxy)butanoic acid ethyl ester, 17 g (0.065 mol) of diethylene glycol dimesylate and 3.6 g (0.026 mol) of anhydrous potassium carbonate in 80 ml of anhydrous acetone and 40 ml of anhydrous dimethylformamide was stirred at reflux for 20 hours. An additional 1.8 g of potassium carbonate was added and reflux was continued for a total of 44 hours. The reaction mixture was filtered and concentrated in vacuo to an orange oil which was treated with ethyl acetate and sodium chloride solution. The yellow oil obtained on concentration of the ethyl acetate was purified by HPLC, eluting with 15% ethyl acetate/toluene to yield 4.1 g (67% yield) of 4-[4-acetyl-3-[2-[2-[(methylsulfonyl)oxy]ethoxy]-ethoxy]-2-propylphenoxy]butanoic acid ethyl ester as a yellow oil.

WORKUP

后处理

  1. temperatureat reflux for 20 hours
  2. temperaturereflux
  3. customwas continued for a total of 44 hours
  4. filtrationThe reaction mixture was filtered
  5. concentrationconcentrated in vacuo to an orange oil which
  6. additionwas treated with ethyl acetate and sodium chloride solution
  7. customThe yellow oil obtained on concentration of the ethyl acetate
  8. customwas purified by HPLC
  9. washeluting with 15% ethyl acetate/toluene