HRID972234

反应详情

EQUATION

反应方程式

HRID 972234 的结构方程式

PROCEDURE

实验过程

The solution of 8 g of crude 2-methyl-4-(6-carbomethoxyhexyl)-thiazole-5-carboxylic acid methylester (VIII, R1 = CH3) in 25 ml of ethanol was treated with 40 ml of 2 N sodium hydroxide solution. The reaction mixture was refluxed for 30 minutes, then acidified with 5 N sulphuric acid under ice-cooling. After extracting the aqueous reaction mixture with 3 × 75 ml of ethyl acetate, the extract was dried over sodium sulphate and evaporated in vacuo. The obtained crude product was recrystallized from a mixture of acetone and n-hexane, affording 5.3 g of 2-methyl-4-(6-carboxyhexyl)-thiazole-5-carboxylic acid (IX, R1 = CH3). M.p.: 147-149° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 30 minutes
  2. temperaturecooling
  3. extractionAfter extracting the aqueous reaction mixture with 3 × 75 ml of ethyl acetate
  4. dry with materialthe extract was dried over sodium sulphate
  5. customevaporated in vacuo
  6. customThe obtained crude product
  7. customwas recrystallized from a mixture of acetone and n-hexane