Process for synthesizing effective azolylamine derivative
A technology for pyrrole amine and derivatives is applied in the field of effective synthesis of pyrrole amine derivatives, which can solve the problems of low reaction yield, difficult purification of target products, expensive production and the like, and achieves the effect of broad application prospects.
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[0042] The following examples help to understand the present invention, but do not limit the content of the present invention.
[0043] Embodiment --- the general operating procedure of reaction
[0044] Synthesis of pyrrolamine derivatives 3 or 4: In a clean reaction tube (without any anhydrous and oxygen-free treatment), add methylenecyclopropanylaldehyde (1, 0.20mmol), hydrazide or hydrazine hydrate (2, 0.4mmol), heated to 110°C in toluene to react for ten minutes. Flash column chromatography (SiO 2 , the eluent is ethyl acetate / petroleum ether=1 / 6) to obtain the corresponding product 3 or 4.
[0045] Product 3a. White solid, melting point: 193-195°C. 1 H NMR (CDCl 3 , 300MHz, TMS) δ 2.10(s, 3H, CH 3 ), 6.11(d, J=3.0Hz, 1H, CH), 6.64(d, J=3.0Hz, 1H, CH), 7.24-7.37(m, 7H, Ar), 7.46-7.51(m, 1H, Ar ), 7.60(d, J=7.5Hz, 1H, Ar), 8.76(s, 1H, NH); 13 C NMR (CDCl 3 , 75MHz, TMS).δ 12.2, 109.4, 116.0, 121.7, 127.1, 127.3, 128.2, 128.7, 129.6, 130.4, 130.9, 131.7, 132.3, 167....
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