反応 #2006462

反応方程式

ethyl acetate

sodium hydride

2,5-dimethyl-4-hydroxyaniline

3-(tert-butyl)-5-chloro-1,2,4-thiadiazole

→

4-[(3-(tert-Butyl)-1,2,4-thiadiazol-5-yl)oxy]-2,5-dimethylaniline

収率 90.0%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   workup.ADDITIONare added
2. 2
   温度cooled down to AT
3. 3
   抽出the solution is extracted three times with water
4. 4
   乾燥dried over MgSO4
5. 5
   その他the solvent is removed under vacuum (1.46 g, 94% purity, 90% yield, log P (pH 2.3)=3.29)

実験手順

754 mg (5.50 mmol) of 2,5-dimethyl-4-hydroxyaniline are dissolved in 5 ml of N,N-dimethylformamide and slowly treated with 242 mg (6.05 mmol) of sodium hydride. The reaction mixture is stirred for 15 min, before 972 mg (5.50 mmol) of 3-(tert-butyl)-5-chloro-1,2,4-thiadiazole are added. Subsequently, the reaction mixture is heated at 100° C. for 1 h and then cooled down to AT. After addition of 20 ml of ethyl acetate, the solution is extracted three times with water and dried over MgSO4, and the solvent is removed under vacuum (1.46 g, 94% purity, 90% yield, log P (pH 2.3)=3.29).

出典