반응 #2006462

반응 방정식

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

수율 90.0%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONare added
2. 2
   온도cooled down to AT
3. 3
   추출the solution is extracted three times with water
4. 4
   건조dried over MgSO4
5. 5
   기타the solvent is removed under vacuum (1.46 g, 94% purity, 90% yield, log P (pH 2.3)=3.29)

실험 절차

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).

출처