HRID972240

反应详情

EQUATION

反应方程式

HRID 972240 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a suspension of 912 mg of 2-methyl-4-(6-carbomethoxyhexyl)-5-(3-keto-1-trans-octenyl)-thiazole (Ia, R1 = CH3) in 20 ml of 0.2 M phosphate buffer of pH 7.5, 90 mg of the lipase enzyme specified in Example 5, 9 mg of the sodium salt of taurocholic acid nd 0.9 ml of a 10 % solution of gum arabic were added. The mixture was then shaken at 25° C in a screening shaker desk at 260 revolutions/minute and an amplitude of 2 cm for 24 hours. Then the reaction mixture was diluted with 50 ml of water, acidified with citric acid and extracted with 3 × 40 ml of ethyl acetate. The ethyl acetate extract was dried over sodium sulphate and evaporated in vacuo. The obtained 1.03 g of evaporation residue were purified by preparative thin layer chromatography in the way specified in Example 6. Thus, 645 mg of 2-methyl-4-(6-carboxyhexyl)-5-(3-keto-1-trans-octenyl)-thiazole Ib, R1 = CH3) were obtained.

WORKUP

后处理

  1. additionwere added
  2. extractionextracted with 3 × 40 ml of ethyl acetate
  3. extractionThe ethyl acetate extract
  4. dry with materialwas dried over sodium sulphate
  5. customevaporated in vacuo
  6. customThe obtained 1.03 g of evaporation residue
  7. customwere purified by preparative thin layer chromatography in the way