Diethyl Ether → HCID 19775941, compound

Participants

Reaction Steps

The dinitrobenzene obtained in Step A (10.0 g, 27.3 mmol) was dissolved in dimethylformamide (40 cm3). Triethylamine (4.6 cm3, 32.7 mmol) and DL 2-aminopropanol (2.6 cm3, 32.7 mmol) were added, and the mixture stirred at room temperature for 17 hours, then at 50° C. for 4 hours. The mixture was cooled to room temperature, poured into diethyl ether (200 cm3) and washed with water (3×200 cm3). The ether layer was collected, dried (MgSO4), filtered and the solvent removed under reduced pressure to give a waxy yellow solid. Recrystallisation (ethyl acetate/hexane) gave DL-2-[5-(4-chloro-1-methyl-5-trifluoromethyl-1H-pyrazol -3-yloxy)-2-nitrophenylamino]-propane-1-ol (8.71 g) as an orange solid. m.p. 118°-120° C.

Provenance & Evidence