A kind of preparation method of α-cyanoamine
A technology of cyanoamine and cyanoacetic acid, which is applied in the preparation of organic compounds, carboxylic acid nitrile preparation, chemical instruments and methods, etc., can solve the problems affecting the safety of the experiment, the low utilization rate of atoms, environmental pollution and other problems, and achieve the goal of reaction Good activity, beneficial to purification, simple post-treatment effect
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Embodiment 1
[0027]
[0028] The reaction vial was filled with TBAI (0.3 mmol, 111 mg), compound 1a (2 mmol, 214 mg), compound 2 (4 mmol, 341 mg), NaOAc (4 mmol, 164 mg), TBHP (0.6 mL), Water (4.0 mL), Tetrahydrofuran (4.0 mL). Then the system was heated at 80 °C in air for about 12 hours, quenched with saturated sodium sulfite solution, extracted with ethyl acetate (40 mL × 3), adsorbed on silica gel, and the product 3a was obtained by simple column chromatography, The yield was 84%. The main test data of the obtained product are as follows. It can be seen from the analysis that the actual synthesized product is consistent with the theoretical analysis.
[0029] 1 H NMR (400 MHz, CDCl 3 ) δ 7.32 – 7.28 (m, 2H), 6.93 – 6.84 (m, 3H), 4.12 (s, 2H), 2.97 (s, 3H); 13 C NMR (100 MHz, CDCl 3 ) δ 147.7, 129.4, 120.1,115.5, 114.8, 42.1, 39.1; MS (ESI-quadrupole): Anal. Calcd. For C 9 h 10 N 2 +H + :147, Found: 147 (M+H + ); IR (neat, cm -1 ): υ 2960, 2891, 2237, 1599, 1500.
Embodiment 2
[0031]
[0032] The reaction vial was filled with TBAI (0.3 mmol, 111 mg), compound 1a (2 mmol, 214 mg), compound 2 (4 mmol, 341 mg), NaOAc (4 mmol, 164 mg), TBHP (0.6 mL), Water (4.0 mL), Tetrahydrofuran (4.0 mL). Then the system was heated at 90°C in air for about 12 hours, quenched with saturated sodium sulfite solution, extracted with ethyl acetate (40 mL × 3), adsorbed on silica gel, and the product 3a was obtained by simple column chromatography, The yield is 80%. The main test data of the obtained product are as follows. It can be seen from the analysis that the actual synthesized product is consistent with the theoretical analysis.
[0033] 1 H NMR (400 MHz, CDCl 3 ) δ 7.32 – 7.28 (m, 2H), 6.93 – 6.84 (m, 3H), 4.12 (s, 2H), 2.97 (s, 3H); 13 C NMR (100 MHz, CDCl 3 ) δ 147.7, 129.4, 120.1,115.5, 114.8, 42.1, 39.1; MS (ESI-quadrupole): Anal. Calcd. For C 9 h 10 N 2 +H + :147, Found: 147 (M+H + ); IR (neat, cm -1 ): υ 2960, 2891, 2237, 1599, 1500.
Embodiment 3
[0035]
[0036]The reaction vial was filled with TBAI (0.3 mmol, 111 mg), compound 1a (2 mmol, 214 mg), compound 2 (4 mmol, 341 mg), NaOAc (4 mmol, 164 mg), TBHP (0.6 mL), Water (4.0 mL), Tetrahydrofuran (4.0 mL). Then the system was heated at 100 °C in air for about 12 hours, quenched with saturated sodium sulfite solution, extracted with ethyl acetate (40 mL × 3), adsorbed on silica gel, and the product 3a was obtained by simple column chromatography, The yield was 77%. The main test data of the obtained product are as follows. It can be seen from the analysis that the actual synthesized product is consistent with the theoretical analysis.
[0037] 1 H NMR (400 MHz, CDCl 3 ) δ 7.32 – 7.28 (m, 2H), 6.93 – 6.84 (m, 3H), 4.12 (s, 2H), 2.97 (s, 3H); 13 C NMR (100 MHz, CDCl 3 ) δ 147.7, 129.4, 120.1,115.5, 114.8, 42.1, 39.1; MS (ESI-quadrupole): Anal. Calcd. For C 9 h 10 N 2 +H + :147, Found: 147 (M+H + ); IR (neat, cm -1 ): υ 2960, 2891, 2237, 1599, 1500.
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