A kind of synthetic method of 1-methyl-2-cyano-3-aliphatic substituted azacene compound
A synthesis method and compound technology, applied in organic chemistry and other directions, can solve the problems of low Ecoscale index, inability to promote industrial application, low atom utilization rate, etc., to improve environmental index, improve atom utilization rate and efficiency, improve yield and The effect of purity
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Embodiment 1~3
[0056] Following examples 1~3 all react by following reaction equation:
[0057]
[0058] The specific operation steps are: in a 50mL pressure-resistant tube, add octyne (30mmol), trimethylcyanosilane (30mmol, 2.97g), N,N-dimethylformamide (30mmol, 2.19g), iodine ammonium chloride (9mmol, 1.30g), and the resulting mixture was stirred and reacted at 100°C for about 3 hours. After the reaction, add 15ml of saturated sodium sulfite to wash, extract 3 times with 15mL of ethyl acetate, combine the extracts, concentrate the extracts in vacuo, and dry in vacuo to calculate the weight.
Embodiment 1
[0060] raw material: Target product:
[0061] 3-hexyl-1-methyl-1H-pyrrole-2-carbonitrile:
[0062] Yield: 92%.
[0063] Yellowish green oil;
[0064] 1 H NMR (500MHz, CDCl 3 )δ6.68(d, J=2.5Hz, 1H), 5.99(d, J=2.5Hz, 1H), 3.71(s, 3H), 2.56(t, J=7.7Hz, 2H), 1.59-1.50( m,4H),1.31-1.30(m,2H),1.30-1.29(m,2H),0.89(t,J=6.7Hz,3H).
[0065] 13 C NMR (126MHz, CDCl 3 )δ137.61, 127.19, 114.09, 109.26, 103.05, 35.37, 31.73, 30.65, 29.01, 26.85, 22.74, 14.23.
[0066] IR (neat, cm –1 )ν2970, 2260, 1555, 1320, 1041, 886, 761, 738.
[0067] HRMS (ESI) calcd for C 9 h 19 N 2 [M+H] + :191.1543, found 191.1546.
Embodiment 2
[0069] raw material: Target product:
[0070] 3-benzyl-1-methyl-1H-pyrrole-2-carbonitrile:
[0071] Yield: 82%.
[0072] 1 H NMR (500MHz, CDCl 3 )δ7.29(t, J=7.5Hz, 2H), 7.25-7.19(m, 3H), 6.69(d, J=2.4Hz, 1H), 5.96(d, J=2.4Hz, 1H), 3.91( s,2H),3.73(s,3H).
[0073] 13 C NMR (126MHz, CDCl 3 )δ140.23, 135.72, 128.67, 128.64, 127.49, 126.41, 113.81, 109.81, 103.30, 35.46, 33.16.
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