Preparation method of beta-amino acetal
A technology of amino acetal and amine acetal, which is applied in the field of preparation of β-amino acetal, can solve the problems of complex operation, poor substrate adaptability, low yield, etc., and achieve simple synthesis process, mild reaction conditions, and reaction selection  good sex effect
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Embodiment 1
[0028] Embodiment 1, β -amino acetal 4a preparation of
[0029]
[0030] n-butyl vinyl ether 1a (80 mg, 0.8 mmol), Pd(Xantphos)Cl 2 (15.1 mg, 5 mol %, 0.02 mmol), amine acetal 2a (164.2 mg, 0.4 mmol) and isopropanol (1.5 mL) were added to the reaction flask, 110 o Reaction under C condition for 12 hours, column chromatography separation (using silica gel column; eluent: petroleum ether / ethyl acetate=100 / 1), to obtain pure product β -amino acetal 4a . The product was a colorless liquid with a yield of 74%. 1 H NMR (400 MHz, CDCl 3 ) δ 7.30-7.35 (m, 4H), 7.22-7.29 (m, 4H), 7.19-7.21 (m, 2H), 4.55 (t, J = 5.6 Hz, 1H), 3.71-3.77 (m, 1H), 3.54 (s, 4H), 3.39-3.44 (m, 1H), 3.23-3.29 (m, 1H), 2.46-2.56 (m, 2H), 1.74-1.86 (m, 2H), 1.38-1.45 (m, 2H), 1.23-1.32 (m, 2H), 1.13 (d, J = 6.0 Hz, 3H), 1.00 (d, J = 6.0 Hz, 3H), 0.87 (t, J = 7.2 Hz, 3H); 13 C NMR (100 MHz, CDCl 3for C 24 h 36 NO 2 [M+H]: 370.2741, found: 370.2747.
Embodiment 2
[0031] Embodiment 2, β -amino acetal 4a preparation of
[0032]
[0033] n-butyl vinyl ether 1a (80 mg, 0.8 mmol), Pd(Xantphos)(CH 3 EN) 2 (OTf) 2 (21.3 mg, 5 mol %, 0.02 mmol), amine acetal 2a (164.2 mg, 0.4 mmol) and isopropanol (1.5 mL) were added to the reaction flask, 110 o Reaction under C condition for 12 hours, column chromatography separation (using silica gel column; eluent: petroleum ether / ethyl acetate=100 / 1), to obtain pure product β -amino acetal 4a . The product was a colorless liquid with a yield of 84%.
Embodiment 3
[0034] Embodiment 3, β -amino acetal 4a preparation of
[0035]
[0036] n-butyl vinyl ether 1a (80 mg, 0.8 mmol), Pd(Xantphos)(CH 3 EN) 2 (OTf) 2 (21.3 mg, 5 mol %, 0.02 mmol), amine acetal 2a (164.2 mg, 0.4 mmol), isopropanol (240 mg, 4 mmol) and toluene (1.5 mL) were added to the reaction flask, 110 o Reaction under C condition for 12 hours, column chromatography separation (using silica gel column; eluent: petroleum ether / ethyl acetate=100 / 1), to obtain pure product β -amino acetal 4a . The product is a colorless liquid with a yield of 85%.
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