HRID972234
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureThe reaction mixture was refluxed for 30 minutes
- temperaturecooling
- extractionAfter extracting the aqueous reaction mixture with 3 × 75 ml of ethyl acetate
- dry with materialthe extract was dried over sodium sulphate
- customevaporated in vacuo
- customThe obtained crude product
- customwas recrystallized from a mixture of acetone and n-hexane