反应 #1880951

反应方程式

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

收率 48.8%

溶剂

DMF

反应条件

后处理

1. 1
   workup.WAITat RT for 48 h
2. 2
   萃取extracted with four times 15 ml of CH2Cl2
3. 3
   干燥The combined organic phase is dried over Na2SO4
4. 4
   过滤filtered
5. 5
   浓缩concentrated
6. 6
   其他Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent

实验过程

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.

来源