Sodium Carbonate → 1-Methyl-4-(3-nitrophenyl)piperazine

참여 물질

반응 단계

A solution of 1-(3-nitrophenyl)piperazine hydrochloride (1.80 g) in water (7 ml) was basified with anhydrous sodium carbonate (0.8 g) and the mixture evaporated to dryness in vacuo. The solid was mixed with formic acid (17 ml) and a solution of formaldehyde 36% in water (1.3 ml, ≡0.47 g CH2O) added and the mixture heated at 95°-98° for 3 h. The mixture was diluted with water (35 ml) and basified with anhydrous sodium carbonate. The suspension was extracted with ethyl acetate (2×80 ml) and the extract dried for 1 h. The mixture was filtered and the filtrate evaporated to dryness to give a dark red oil which was dissolved in ether (20 ml) and filtered. The filtrate was evaporated to dryness to give a red oil which was purified by FCC eluting with System A (500:8:1) to give an orange oil which was dried in vacuo. Upon scratching, crystallisation began and the oil was left to stand until crystallisation of the title compound was complete (1.10 g) m.p. 53°-54° C.

출처 및 근거