반응 #475164

반응 방정식

water

4-Chloro-6-(4-nitrophenoxy)pyrimidine

ammonia ethanol

ethyl acetate

ethyl acetate

→

title compound

수율 33.0%

6-(4-Nitrophenoxy)pyrimidin-4-ylamine

수율 33.0%

용매

hexane

반응 조건

후처리

1. 1
   세척the organic layer was washed with 1N aqueous sodium hydroxide, water and saturated saline
2. 2
   건조dried over anhydrous magnesium sulfate
3. 3
   여과the drying agent was filtered off
4. 4
   workup.DISTILLATIONthe filtrate was distilled off under reduced pressure
5. 5
   기타The obtained crude product
6. 6
   workup.ADDITIONthe fraction containing the target substance
7. 7
   농축was concentrated

실험 절차

4-Chloro-6-(4-nitrophenoxy)pyrimidine (1.04 g, 4.00 mmol) was heated and stirred in an ammonia-ethanol solution (14%, 10 ml) at 110° C. for 15 minutes using an autoclave. The reaction solution was distributed between ethyl acetate and water, the organic layer was washed with 1N aqueous sodium hydroxide, water and saturated saline and dried over anhydrous magnesium sulfate, the drying agent was filtered off and the filtrate was distilled off under reduced pressure. The obtained crude product was subjected to silica gel column chromatography (eluent-ethyl acetate:hexane=1:1), and the fraction containing the target substance was concentrated to obtain the title compound (306 mg, 1.32 mmol, 33%) as colorless crystals.

출처