反应 #2460281

反应方程式

ether

methoxyethoxymethyl chloride

4-iodophenol

sodium hydride

→

4-Methoxyethoxymethoxy-iodobenzene

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   温度warmed to room temperature
2. 2
   workup.STIRRINGstirred for 24 hours
3. 3
   其他The solvent was removed under reduced pressure
4. 4
   洗涤washed with 5% sodium hydroxide (4×200 ml), water (4×200 ml), saturated sodium chloride (1×200 ml)
5. 5
   干燥dried over sodium sulfate
6. 6
   其他Evaporation of the solvent under reduced pressure
7. 7
   其他gave an oily product in 14.1 g

实验过程

A solution of 4-iodophenol (10 g, 45.45 mmol) in 200 ml of anhydrous tetrahydrofuran was treated at 0° C. with sodium hydride (2.36 g, 60% dispersion, 59.09 mmol) for 5 minutes. To the resulting mixture, methoxyethoxymethyl chloride (8.3 ml, 72.73 mmol) was slowly added over a 5-minute period. The mixture was stirred at 0° C. under nitrogen for 30 minutes, warmed to room temperature, and stirred for 24 hours. The solvent was removed under reduced pressure. The residue was taken into 500 ml of ether, washed with 5% sodium hydroxide (4×200 ml), water (4×200 ml), saturated sodium chloride (1×200 ml), and dried over sodium sulfate. Evaporation of the solvent under reduced pressure gave an oily product in 14.1 g. TLC (silica gel, ether): Rf 0.5.

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