反応 #2166380

反応方程式

1-fluoro-2-iodoethane

1g

2-{3-[(4-carbamimidoylphenylamino)-(2-fluoro-4,5-dimethoxyphenyl)methyl]5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl}benzoic Acid trifluoroacetate

5-methoxy-1,3-benzenedimethanol

sodium hydride

→

title compound

[3-(2-fluoro ethoxymethyl)-5-methoxyphenyl]methanol

溶媒

DMF

ethyl acetate

Water

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 22 hours
2. 2
   洗浄The organic layer was washed with water and saturated brine
3. 3
   乾燥dried over anhydrous sodium sulfate
4. 4
   ろ過The desiccating agent was filtered off
5. 5
   濃縮the filtrate was concentrated under reduced pressure
6. 6
   その他The residue was purified by silica gel column chromatography (ethyl acetate-heptane)

実験手順

To a solution of 1g of 5-methoxy-1,3-benzenedimethanol in 10 ml of DMF there was added 238 mg of sodium hydride (60% oily suspension) at 0° C. After stirring at room temperature for 30 minutes, 1.04 g of 1-fluoro-2-iodoethane was added and the mixture was stirred at room temperature for 22 hours. Water was added to the reaction mixture and extraction was performed with ethyl acetate. The organic layer was washed with water and saturated brine, and then dried over anhydrous sodium sulfate. The desiccating agent was filtered off and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate-heptane) to give the title compound (145 mg) as a colorless oil.

出典