反应 #1583812

反应方程式

ethyl acetate

2-isopropyl-4-(4-fluorophenyl)-1,3-thiazole

4-bromo-2-methylpyridine

potassium acetate

→

4-[4-(4-Fluorophenyl)-2-isopropyl-1,3-thiazol-5-yl]-2-methylpyridine

溶剂

DMA

反应条件

后处理

1. 1
   过滤the reaction mixture is filtered through a silica gel cartridge
2. 2
   workup.ADDITION10 ml of water are added to the filtrate
3. 3
   其他The organic phase is separated off
4. 4
   洗涤washed once more with 10 ml of water
5. 5
   干燥dried over MgSO4
6. 6
   浓缩concentrated under reduced pressure
7. 7
   其他The residue is purified by column chromatography on silica gel (cyclohexane/ethyl acetate)

实验过程

Under argon, 200 mg (0.90 mmol) of 2-isopropyl-4-(4-fluorophenyl)-1,3-thiazole, 77 mg (0.45 mmol) of 4-bromo-2-methylpyridine, 133 mg (1.35 mmol) of potassium acetate and 0.4 mg (2 μmol) of palladium(II) acetate in 5 ml of DMA are heated to 150° C. After 3 h, 50 ml of ethyl acetate are added and the reaction mixture is filtered through a silica gel cartridge. 10 ml of water are added to the filtrate. The organic phase is separated off, washed once more with 10 ml of water, dried over MgSO4 and concentrated under reduced pressure. The residue is purified by column chromatography on silica gel (cyclohexane/ethyl acetate). This gives 115 mg (41%) of the desired product; 1H-NMR(DMSO-(D6) δ: 8.39 (d, 1H), 7.48 (m, 2H), 7.22 (m, 2H), 7.17 (s, 1H), 7.03 (d, 1H), 3.35 (m, 1H), 2.43 (s, 3H), 1.39 (d, 6H).

来源