反应详情

A stirred solution of methyl 5-chloro-2-nitro-benzoate (17.0 g., 0.079 mole) and the potassium salt of 2,4,6-trichlorophenol (18.6 g., 0.079 mole) in dimethyl sulfoxide (100 ml.) was heated at 90° C. for 17 hours. The cooled reaction mixture was diluted with water (500 ml.) and then extracted with ether (3×100 ml.). The combined ether fractions were washed with 10% sodium hydroxide solution (2×30 ml.) and then with a saturated aqueous chloride solution. The ether solution was dried (Na2SO4) and the solvent evaporated to give a dark oil. Two crystallizations (petroleum ether) gave 1.91 g. of a pale yellow solid, m.p. 101°-103° C.

1. customThe cooled reaction mixture
2. extractionextracted with ether (3×100 ml.)
3. washThe combined ether fractions were washed with 10% sodium hydroxide solution (2×30 ml.)
4. dry with materialThe ether solution was dried (Na2SO4)
5. customthe solvent evaporated
6. customto give a dark oil
7. customTwo crystallizations (petroleum ether)
8. customgave 1.91 g