반응 #1880951

반응 방정식

water

5-methyl-4-methylsulfonyl-2-(4-trifluoromethyl-1H-1-pyrazolyl)pyrimidine

3-hydroxy-5-trifluoromethylthiophene

K2CO3

→

5-methyl-2-(4-trifluoromethyl-1H-1-pyrazolyl)-4-(5-trifluoromethyl-3-thienyloxy)pyrimidine

수율 48.8%

용매

DMF

반응 조건

후처리

1. 1
   workup.WAITat RT for 48 h
2. 2
   추출extracted with four times 15 ml of CH2Cl2
3. 3
   건조The combined organic phase is dried over Na2SO4
4. 4
   여과filtered
5. 5
   농축concentrated
6. 6
   기타Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent

실험 절차

A mixture of 0.8 g (2.6 mmol) of 5-methyl-4-methylsulfonyl-2-(4-trifluoromethyl-1H-1-pyrazolyl)pyrimidine, 0.44 g (2.6 mmol) of 3-hydroxy-5-trifluoromethylthiophene and 0.72 g (5.2 mmol) of K2CO3 in 10 ml of DMF is stirred at 60° C. for 6 h and then at RT for 48 h. It is subsequently poured into 20 ml of water and extracted with four times 15 ml of CH2Cl2. The combined organic phase is dried over Na2SO4, filtered and concentrated. Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent gives 0.5 g of 5-methyl-2-(4-trifluoromethyl-1H-1-pyrazolyl)-4-(5-trifluoromethyl-3-thienyloxy)pyrimidine as colorless crystals.

출처