Sodium Iodide → 2,4-Dichloro-6-iodophenol

To a solution of 6.52 g (40 mmol) of 2,4-dichlorophenol and 7.76 g (52 mmol) of sodium iodide in 80 mL of acetonitrile and 16 mL of water at room temperature add 5.64 g (52 mmol) of tert-butyl hypochlorite dropwise over a period of 30 minutes. Stir the reaction mixture for 3 hours at ambient temperature. Dilute the reaction mixture with 200 mL of ethyl acetate. Wash the resulting organic solution successively with 5% aqueous sodium thiosulfate solution and brine and dry over anhydrous magnesium sulfate. Remove the solvent and then crystallize from hexanes to yield 5.9 g (51%) of (P9) as a slightly colored solid.

1. washWash the resulting organic solution successively with 5% aqueous sodium thiosulfate solution and brine
2. dry with materialdry over anhydrous magnesium sulfate
3. customRemove the solvent
4. customcrystallize from hexanes
5. customto yield 5.9 g (51%) of (P9) as a slightly colored solid

ORD-Eintrag

ord-aa4e557fd0d446c8accf1c8b41225f23

Quelldatensatz

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09000108B2