반응 #1445500

반응 방정식

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

4-tert.-butylbenzene sulfonamide potassium salt

water

→

4-tert.-butyl-N-[6-chloro-5-(p-tolyl)-4-pyrimidinyl]-benzene sulfonamide

수율 96.3%

용매

DMSO

반응 조건

후처리

1. 1
   추출extracted twice with 100 ml of diethyl ether
2. 2
   추출The organic layers was extracted twice with 50 ml of water
3. 3
   추출The resulting fine suspension was extracted twice with ethyl acetate
4. 4
   건조The combined organic layers was dried over Na2SO4
5. 5
   기타evaporated
6. 6
   기타The residue was dried under high vacuum

실험 절차

A mixture of 0.8 g of 4,6-dichloro-5-(p-tolyl)-pyrimidine and 1.68 g of 4-tert.-butylbenzene sulfonamide potassium salt in 20 ml of DMSO was stirred at room temperature for 24 h. The mixture was poured onto 200 ml of water and extracted twice with 100 ml of diethyl ether. The organic layers was extracted twice with 50 ml of water. The combined aqueous layers was acidified with conc. hydrochloric acid. The resulting fine suspension was extracted twice with ethyl acetate. The combined organic layers was dried over Na2SO4 and evaporated. The residue was dried under high vacuum to give 1.34 g 4-tert.-butyl-N-[6-chloro-5-(p-tolyl)-4-pyrimidinyl]-benzene sulfonamide as a white powder. LC-MS: tR=5.92 min, [M+1]+=416.20, [M−1]−=414.24.

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