反応 #450292

反応方程式

3-chloro-4-methoxymethoxy-5-methylphenol

potassium carbonate

1,1,3-trichloro-1-propene

→

3-chloro-4-methoxymethoxy-5-methyl-1-(3,3-dichloro-2-propenyloxy)benzene

収率 91.7%

溶媒

N,N-dimethylformamide

N,N-dimethylformamide

反応条件

後処理

1. 1
   workup.STIRRINGAfter stirring at room temperature for 12 hours
2. 2
   抽出extracted with 200 ml of diethyl ether
3. 3
   洗浄The combined ether was washed with water
4. 4
   乾燥dried with anhydrous magnesium sulfate
5. 5
   濃縮concentrated

実験手順

To a mixture of 10 g of 3-chloro-4-methoxymethoxy-5-methylphenol, 7 g of potassium carbonate and 100 ml of N,N-dimethylformamide was added dropwise a solution of 8 g of 1,1,3-trichloro-1-propene dissolved in 30 ml of N,N-dimethylformamide, while stirring at room temperature. After stirring at room temperature for 12 hours, the reaction mixture was poured into ice water, and extracted with 200 ml of diethyl ether. The combined ether was washed with water, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel chromatography, which afforded 14.1 g of 3-chloro-4-methoxymethoxy-5-methyl-1-(3,3-dichloro-2-propenyloxy)benzene (91% yield).

出典