反応 #347955

反応方程式

3,5-dichloro-4-(3-chloro-5-trifluoromethyl-2-pyridyloxy)phenol

potassium carbonate

1,1,3-trichloro-1-propene

→

3,5-dichloro-4-(3-chloro-5-trifluoromethyl-2-pyridyloxy)-1-(3,3-dichloro-2-propenyloxy)benzene

収率 79.2%

溶媒

N,N-dimethylformamide

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 5 hours
4. 4
   抽出extracted twice with 40 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 93 mg of 3,5-dichloro-4-(3-chloro-5-trifluoromethyl-2-pyridyloxy)phenol, 40 mg of potassium carbonate and 10 ml of N,N-dimethylformamide, a solution prepared by dissolving 42 mg of 1,1,3-trichloro-1-propene in 3 ml of N,N-dimethylformamide was added dropwise at room temperature with stirring. After stirring at room temperature for 5 hours, the reaction solution was poured into ice-water, and extracted twice with 40 ml of diethyl ether. Then, the ether layers were combined, washed with water, dried over anhydrous magnesium sulfate and concentrated to give a crude product. This crude product was subjected to silica gel chromatography to give 96 mg of 3,5-dichloro-4-(3-chloro-5-trifluoromethyl-2-pyridyloxy)-1-(3,3-dichloro-2-propenyloxy)benzene, yield 79%; m.p., 97.8° C.

出典