반응 #1052806

반응 방정식

diethylether

4,6-dichloro-5-p-tolyl-pyrimidine

di-isopropyl-ethyl-amine

2-phenyl-ethenesulfonamide potassium salt

→

2-phenyl-ethenesulfonic acid(6-chloro-5-p-tolyl-pyrimidin-4-yl)-amide

수율 62.6%

용매

DMSO

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGthe solution was stirred for 30 minutes
3. 3
   기타The layers were separated
4. 4
   온도cooled to 0° C. for 1 h
5. 5
   여과The precipitated product was filtered off
6. 6
   세척washed with water and diethylether
7. 7
   기타dried

실험 절차

To 4,6-dichloro-5-p-tolyl-pyrimidine (2.0 g) disolved in DMSO (35 ml) was added di-isopropyl-ethyl-amine (1.46 ml) followed by 2-phenyl-ethenesulfonamide potassium salt (2.78 g). The mixture was stirred for 48 h at rt then poured onto water (500 ml) and diethylether (250 ml) was added and the solution was stirred for 30 minutes. The layers were separated and the water layer was acidified with acetic acid (2.0 ml) and cooled to 0° C. for 1 h. The precipitated product was filtered off and washed with water and diethylether and dried to give 2-phenyl-ethenesulfonic acid(6-chloro-5-p-tolyl-pyrimidin-4-yl)-amide (2.02 g). tR=5.32 (LC); M+=386.23 (ES+); M−=384.22 (ES−).

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