2,3-dichloro-4-methoxyphenol

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a suspension of NaH (2.5 g., 0.052 mole of a 50% mineral oil suspension) in 60 ml. of DMF was added portionwise 2,3-dichloro-4-methoxyphenol (9.0 g., 0.047 mole) prepared as described by F. Dallacker and J. Van Wersch, Chem. Ber., 105, 3301 (1972). The mixture was stirred at room temperature under nitrogen for 15 minutes and then p-fluoronitrobenzene was rapidly added. The resulting mixture was heated at 100° for 2.5 hr., cooled to room temperature, and poured into ice water. The precipitate was filtered, washed with methanol and dried to give 13 g. of product, m.p. 165°-166°. prepared The resulting mixture was heated at 100° for 2.5 hr , cooled to room temperature The precipitate was filtered washed with methanol dried to give 13 g