Methyl iodide → HCID 23181677, compound

Participants

Reaction Conditions

Reaction Steps

6.1 g (0.02 mol) of N-(4-chloro-2-fluoro-5-hydroxyphenyl)-3-methyl-3,4,5,6-tetrahydrophthalic acid imide are heated at 80° C. together with 3.0 g (0.022 mol) of potassium carbonate in 50 ml of methyl propyl ketone. After 30 minutes thick salt is precipitated. 1.5 ml (0.024 mol) of methyl iodide are added at 35° C. and the reaction mixture, which is now thinly liquid again, is stirred for 2 hours at 45° C. in order to complete the reaction. The salts are filtered off and the filtrate is concentrated by evaporation and the residue is chromatographed over a small column of silica gel with hexane/ethyl acetate 9:1. After concentration of the main fractions by evaporation there are obtained 4.7 g (73.4%) of the title compound (Compound No. 1.113) of the formula ##STR10## in the form of a clear colourless oil, nD21 =1.412.

Provenance & Evidence