反応 #347963

反応方程式

3,5-dichloro-4-(3-bromo-5-trifiuoromethyl-2-pyridyloxy)phenol

potassium carbonate

1,1,3-trichloro-1-propene

→

3,5-dichloro-4-(3-bromo-5-trifluoromethyl-2-pyridyloxy)-2-(3,3-dichloro-2-propenyloxy)benzene

収率 75.0%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   その他a solution prepared
2. 2
   workup.ADDITIONwas added dropwise at room temperature
3. 3
   workup.STIRRINGAfter stirring at room temperature for 7 hours
4. 4
   抽出extracted twice with 50 ml of diethyl ether
5. 5
   洗浄washed with water
6. 6
   乾燥dried over anhydrous magnesium sulfate
7. 7
   濃縮concentrated
8. 8
   その他to give a crude product

実験手順

To a mixture of 0.83 g of 3,5-dichloro-4-(3-bromo-5-trifiuoromethyl-2-pyridyloxy)phenol, 0.31 g of potassium carbonate and 20 ml of N-dimethylformamide, a solution prepared by dissolving 0.33 g of 1,1,3-trichloro-1-propene in 5 ml of N,N-dimethylformamide was added dropwise at room temperature with stirring. After stirring at room temperature for 7 hours, the reaction solution was poured into ice-water, and extracted twice with 50 ml of diethyl ether. Then, the ether layers were combined, washed with water, dried over anhydrous magnesium sulfate and then concentrated to give a crude product. This crude product was subjected to silica gel chromatography to give 0.79 g of 3,5-dichloro-4-(3-bromo-5-trifluoromethyl-2-pyridyloxy)-2-(3,3-dichloro-2-propenyloxy)benzene, yield 75%; m.p., 90.7° C.

出典