反応 #631845

反応方程式

sodium hydride

2-bromoformylacetic acid ethyl ester

4,5-bis-(p-methoxyphenyl)-thiazoline-2-thione

sodium

→

2-[4,5-bis-(p-methoxyphenyl)-thiazol-2-ylthio]-2-formylacetic acid ethyl ester

溶媒

diethyl ether

hexane

hexamethylphosphoric acid triamide

反応条件

後処理

1. 1
   温度the solution is cooled to 5°
2. 2
   洗浄The ethereal phase is washed with water
3. 3
   乾燥dried over magnesium sulphate
4. 4
   濃縮concentrated to dryness by evaporation

実験手順

3.3 g of 4,5-bis-(p-methoxyphenyl)-thiazoline-2-thione are dissolved in 50 ml of hexamethylphosphoric acid triamide, the solution is cooled to 5° and converted into the sodium salt under nitrogen with sodium hydride (0.5 g of a 50% strength suspension in mineral oil, de-oiled with hexane). The product is allowed to warm to room temperature, 2.0 g of 2-bromoformylacetic acid ethyl ester are added dropwise and the mixture is stirred at 25° for 1 hour, poured into 750 ml of ice-water and taken up in diethyl ether. The ethereal phase is washed with water, dried over magnesium sulphate and concentrated to dryness by evaporation. 2-[4,5-bis-(p-methoxyphenyl)-thiazol-2-ylthio]-2-formylacetic acid ethyl ester is obtained, which can be used without further purification.

出典