反応 #347957

反応方程式

2-trifluoromethyl-4-(3-ethoxyphenoxy)phenol

1,1,3-trichloro-1-propene

→

2-trifluoromethyl-4-(3-ethoxyphenoxy)-1-(3,3-dichloro-2-propenyloxy)benzene

収率 62.0%

溶媒

sodium hydride

N,N-dimethylformamide

反応条件

後処理

1. 1
   その他To a solution prepared
2. 2
   workup.ADDITIONwas added
3. 3
   その他a solution prepared
4. 4
   workup.ADDITIONwas added dropwise under ice cooling
5. 5
   workup.STIRRINGAfter stirring at room temperature for 10 hours
6. 6
   抽出extracted twice with 50 ml of diethyl ether
7. 7
   洗浄washed with water
8. 8
   乾燥dried over anhydrous magnesium sulfate
9. 9
   濃縮concentrated
10. 10
    その他to give a crude product

実験手順

To a solution prepared by dissolving 0.44 g of 2-trifluoromethyl-4-(3-ethoxyphenoxy)phenol in 10 ml of N,N-dimethylfonnamide, 0.062 g of sodium hydride (60% oil-based) was added with stirring under ice cooling. After 10 minutes, a solution prepared by dissolving 0.24 g of 1,1,3-trichloro-1-propene in 5 ml of N,N-dimethylformamide was added dropwise under ice cooling. After stirring at room temperature for 10 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 concentrated to give a crude product. This crude product was subjected to silica gel chromatography to give 0.37 g of 2-trifluoromethyl-4-(3-ethoxyphenoxy)-1-(3,3-dichloro-2-propenyloxy)benzene, yield 62%; nD23.6 1.5369.

出典