HRID972244

反应详情

EQUATION

反应方程式

HRID 972244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the solution of 353 mg of 4-(6-carbomethoxyhexyl)-5-(3-hydroxy-1-trans-octenyl)-thiazole (Ic, R1 = H) in 4 ml of anhydrous pyridine, 1 ml of acetic anhydride was added. The reaction mixture was allowed to stand for 24 hours at room temperature, diluted with 50 ml of water and extracted with 3 × 15 ml of ethyl acetate. The ethyl acetate extract was washed with water, dried over sodium sulphate and evaporated under vacuum in vacuo. The obtained 390 mg of evaporation residue was purified by preparative thin layer chromatography, using a silica gel layer as adsorbent and a mixture of 40 % ethyl acetate and 60 % n-heptane as running solvent. Thus, 285 mg of 4-(6-carbomethoxyhexyl)-5-(3-acetoxy-1-trans-octenyl)-thiazole (Ie, R1 = H) of chromatographic purity were obtained.

WORKUP

后处理

  1. extractionextracted with 3 × 15 ml of ethyl acetate
  2. extractionThe ethyl acetate extract
  3. washwas washed with water
  4. dry with materialdried over sodium sulphate
  5. customevaporated under vacuum in vacuo
  6. customThe obtained 390 mg of evaporation residue
  7. customwas purified by preparative thin layer chromatography
  8. additiona mixture of 40 % ethyl acetate and 60 % n-heptane