Diethyl Ether → 4-Methoxyethoxymethoxy-iodobenzene

温度

0 °C

A solution of 4-iodophenol (10 g, 45.45 mmoles) in 200 mL of anhydrous tetrahydrofuran was treated at 0° C. with sodium hydride (2.36 g, 60% dispersion, 59.09 mmoles) for 5 minutes. To the resulting mixture was slowly added over a 5 minute period methoxyethoxymethyl chloride (8.3 mL, 72.73 mmoles). The mixture was stirred at 0° C. for 30 minutes, warmed to room temperature, and stirred under nitrogen for 24 hours. The solvent was removed under reduced pressure. The residue was taken into 500 mL of ether, washed with 200 mL of 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.

1. temperaturewarmed to room temperature
2. stirringstirred under nitrogen for 24 hours
3. customThe solvent was removed under reduced pressure
4. washwashed with 200 mL of 5% sodium hydroxide (4×200 mL), water (4×200 mL), saturated sodium chloride (1×200 mL)
5. dry with materialdried over sodium sulfate
6. customEvaporation of the solvent under reduced pressure
7. customgave an oily product in 14.1 g

ORDレコード

ord-f41363a47ca748ff839e0a6c27866b3a

出典データセット

uspto-grants-2009_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07611909B1