反応 #1929004

反応方程式

compound ( 48 )

4-bromo-1-[5-(trifluoromethyl)-2-pyridyl]piperidine

sodium hydride

DMF

compound ( 46 )

2-propoxy-4-(trifluoromethyl)benzenethiol

→

4-[2-propoxy-4-(trifluoromethyl)phenylsulfanyl]-1-[5-(trifluoromethyl)-2-pyridyl]piperidine

溶媒

water

反応条件

後処理

1. 1
   温度was heated to 100° C.
2. 2
   workup.STIRRINGwas then stirred for 1 hour
3. 3
   温度After the mixture was cooled
4. 4
   抽出was then subjected to extraction with ethyl acetate
5. 5
   洗浄After its organic layer was washed with water
6. 6
   乾燥was then dried with anhydrous magnesium sulfate, it
7. 7
   ろ過was filtered
8. 8
   濃縮was then concentrated under reduced pressure
9. 9
   その他Its residue was purified by column chromatography
10. 10
    その他to produce the chemical compound

実験手順

After 60% sodium hydride was added, with chilling on ice, to the DMF (7 ml) solution of the chemical compound (46) (0.62 g), it was warmed to room temperature, and was then stirred for 30 minutes. After the chemical compound (48) (0.74 g) was added to the mixture, it was heated to 100° C., and was then stirred for 1 hour. After the mixture was cooled, it was poured into water, and was then subjected to extraction with ethyl acetate. After its organic layer was washed with water, and was then dried with anhydrous magnesium sulfate, it was filtered, and was then concentrated under reduced pressure. Its residue was purified by column chromatography to produce the chemical compound mentioned in the above title (0.90 g).

出典