반응 #40367

반응 방정식

water

2,5-dichloro-N-ethyl-N-methylpyrimidin-4-amine

4-nitro-2,5-dimethylphenol

potassium carbonate

→

5-chloro-2-(2,5-dimethyl-4-nitrophenoxy)-N-ethyl-N-methylpyrimidin-4-amine

용매

DMF

반응 조건

후처리

1. 1
   추출was extracted twice with 50 ml dichloromethane
2. 2
   세척The combined organic layers were washed with aqueous solution of sodium hydroxide
3. 3
   건조The organic layer was dried over magnesium sulfate
4. 4
   농축concentrated in vacuo and column chromatography (dichloromethane)
5. 5
   기타yielded 8.3 g (47%) with a purity of 76%

실험 절차

A solution of 16.8 g (40 mmol) 2,5-dichloro-N-ethyl-N-methylpyrimidin-4-amine, 7.35 g 4-nitro-2,5-dimethylphenol (44 mmol) and 8.29 g potassium carbonate (60 mmol) in 70 ml DMF were stirred for 20 hrs at 100° C. After adding the mixture to 150 ml water the resulting suspension was extracted twice with 50 ml dichloromethane. The combined organic layers were washed with aqueous solution of sodium hydroxide. The organic layer was dried over magnesium sulfate, concentrated in vacuo and column chromatography (dichloromethane) yielded 8.3 g (47%) with a purity of 76%; log P (pH=2.3)=4.07.

출처