Synthesis
A solution of 5 g (0.02 mol) bicaret in 150 ml of 25% sulfuric acid was boiled for 40 h, then cooled to 20°C and neutralized with 40% sodium hydroxide solution. The resulting inorganic salt precipitate was separated, and the filtrate was evaporated to dryness. The residue was dried with 50 ml of ethanol, the inorganic layer was filtered, and the ethanol-water filtrate was evaporated to dryness. The residual water was removed with benzene (4 × 50 ml). The residue produced by distillation was obtained. The residue was crystallized from a mixture of chloroform and diethyl ether (1:1) to give the substance. The hydrolysis product of compound I was formed, and its composition and structure were studied using elemental analysis and PMR spectroscopy. Yield: 2.1 g (70%) and 1,3-diethylurea, yield: 1.2 g (55%). Product ratio: 1:1. Compound II: (boiling point 120-121°C/3 mmHg). Elemental analysis: Carbon content is 53.5%, hydrogen content is 7.6%, C7H12N2O2, calculated value: carbon content 53.8%, hydrogen content 7.6%. PMR spectral parameters: -CH3(Et): 1.25(t), 6H, -CH2-(Et): 1.1(t), 6h, -CH2-(5): 3.56(m), 4H. Compound III: Melting temperature is 109-110℃. Elemental analysis: Elemental composition: 51.6%H, 10.3%H; C5H12N2O; calculated: 51.7%C, 10.3%H. PMR spectral parameters: -CH3(Et): 3.13(q), 4H, -CH2-(Et): 4.92(s), 2H.
Figure 1,3-Diethylurea
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