A kind of synthetic method of α-acyloxycarbonyl compound
A synthesis method and compound technology, applied in the preparation of organic compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve harsh reaction conditions, product yields are not high enough, substrate types Limitations and other issues, to achieve the effect of efficient preparation and accelerated reaction process
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Embodiment 1
[0038]
[0039]Add 1 mol formula (I) compound, 2.3 mol formula (II) compound and 12L acetonitrile in the reactor, stir and mix evenly, then add 0.4 mol methyltriphenylphosphine iodide, containing 5.8 mol TBHP with a mass concentration of 70% TBHP aqueous solution and a mixture of triethanolamine borate and sodium citrate with a mass ratio of 1:1.1 (the total mass is 23g), after sealing, stir and heat up to 85°C for 14h, after the reaction is completed, cool to room temperature, and concentrate in vacuo. The residue was purified by silica gel column chromatography to obtain the compound of formula (III) with a yield of 96.6% and a purity of 99.1% (HPLC).
[0040] 1 H NMR (300MHz, CDCl 3 )δ1.65(d, J=7.2Hz, 3H), 6.17(q, J=7.2Hz, 1H), 7.47-7.52(m, 2H), 7.58-7.63(m, 3H), 7.95-8.01(m ,4H);
[0041] MS[M+Na] + : 354.98.
Embodiment 2
[0043]
[0044] Add 1mol of the compound of formula (I), 2.5mol of the compound of formula (II) and 15L of acetonitrile in the reactor, stir and mix evenly, then add 0.3mol of methyltriphenylphosphine iodide, containing 5.5mol of TBHP at a mass concentration of 70% TBHP aqueous solution and a mixture of triethanolamine borate and sodium citrate with a mass ratio of 1:1.1 (the total mass is 20g), after sealing, stir and heat up to 90°C for 15h, after the reaction is completed, cool to room temperature, and concentrate in vacuo , and the residue was purified by silica gel column chromatography to obtain the compound of formula (III) with a yield of 94.7% and a purity of 98.9% (HPLC).
[0045] 1 H NMR (300MHz, CDCl 3 )δ1.64(d, J=7.2Hz, 3H), 2.57(s, 3H), 6.21(q, J=6.9Hz, 1H), 7.22-7.26(m, 2H), 7.36-7.60(m, 4H ), 8.01-8.03 (m, 3H);
[0046] MS[M+H] + : 269.11.
Embodiment 3
[0048]
[0049] Add 1 mol formula (I) compound, 2.2 mol formula (II) compound and 10L acetonitrile in the reactor, stir and mix evenly, then add 0.5 mol methyltriphenylphosphine iodide, containing 5.7 mol TBHP mass concentration is 70% TBHP aqueous solution and a mixture of triethanolamine borate and sodium citrate with a mass ratio of 1:1.1 (the total mass is 25g), after sealing, stir and heat up to 80°C for 13h of reaction, after the reaction is completed, cool to room temperature, and concentrate in vacuo. The residue was purified by silica gel column chromatography to obtain the compound of formula (III) with a yield of 94.5% and a purity of 99.2% (HPLC).
[0050] 1 H NMR (300MHz, CDCl 3 )δ1.70(d, J=7.2Hz, 3H), 6.23(q, J=7.2Hz, 1H), 7.41-7.47(m, 3H), 7.55-7.61(m, 1H), 7.84(t, J =7.7Hz, 1H), 7.98-8.02(m, 2H), 8.12-8.15(m, 1H), 8.75-8.76(m, 1H);
[0051] MS[M+H] + : 256.09.
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