تفاعل #1583812

معادلة التفاعل

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

المذيبات

DMA

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe reaction mixture is filtered through a silica gel cartridge
2. 2
   workup.ADDITION10 ml of water are added to the filtrate
3. 3
   أخرىThe organic phase is separated off
4. 4
   غسيلwashed once more with 10 ml of water
5. 5
   تجفيفdried over MgSO4
6. 6
   تركيزconcentrated under reduced pressure
7. 7
   أخرىThe residue is purified by column chromatography on silica gel (cyclohexane/ethyl acetate)

الإجراء التجريبي

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).

المصدر