反応 #631829

反応方程式

sodium hydride

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

hydrochloric acid

2-iodoethanol

→

2-(2-hydroxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole

溶媒

hexane

hexamethylphosphoric acid triamide

反応条件

後処理

1. 1
   温度the solution is cooled to 5°
2. 2
   workup.STIRRINGThe mixture is then stirred for 30 minutes at room temperature
3. 3
   workup.STIRRINGthe mixture is then stirred for 15 minutes at room temperature
4. 4
   workup.WAITAfter being left
5. 5
   その他separates crystallises
6. 6
   乾燥The solution is dried over magnesium sulphate
7. 7
   濃縮concentrated to dryness by evaporation
8. 8
   その他To crystallise
9. 9
   その他the residue is triturated with diethyl ether

実験手順

10 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, while stirring, sodium hydride (1.45 g of a 50% strength suspension in mineral oil, de-oiled with hexane) is added. The mixture is then stirred for 30 minutes at room temperature, 5.22 g of 2-iodoethanol are added dropwise thereto, and the mixture is then stirred for 15 minutes at room temperature and poured into a mixture of 30 ml of 2 N hydrochloric acid and 400 ml of ice-water. After being left to stand for some time the oil which separates crystallises and is taken up in 200 ml of methylene chloride. The solution is dried over magnesium sulphate and concentrated to dryness by evaporation. To crystallise, the residue is triturated with diethyl ether. 2-(2-hydroxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole having a melting point of 83°-84° is obtained.

出典