Iodine → 2-IODO-5-METHOXYPHENOL

I2 (40.9 g, 161.1 mmol) was dissolved in CHCl3 (850 mL) with stirring over 1 hour. The solution was added slowly into a reaction mixture of 3-methoxyphenol 5-A (20 g, 161.1 mmol) and silver trifluoroacetate in 200 mL CHCl3 over 1.5 hours. The reaction was stirred at room temperature for 16 hours. Solids were removed by filtration. The filtrate was washed with 5% Na2S2O3(500 mL), saturated NaHCO3, brine, dried over MgSO4 and concentrated. The crude mixture was triturated with carbon tetrachloride to give 2-iodo-5-methoxyphenol 5-B (13.6 g) as a white solid. The remaining crude products were purified by silica gel column chromatography eluted with CH2Cl2to give 28.2 g of compound 5-B.

1. stirringThe reaction was stirred at room temperature for 16 hours
2. customSolids were removed by filtration
3. washThe filtrate was washed with 5% Na2S2O3(500 mL), saturated NaHCO3, brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customThe crude mixture was triturated with carbon tetrachloride

ORDレコード

ord-b48948d38dc0418fa826935f20fc0fa1

出典データセット

uspto-grants-2008_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07381824B2