A kind of preparation method of arylmethyl phosphonate
A technology of arylmethylphosphonate and arylacetic acid, applied in the field of preparation of arylmethylphosphonate, can solve the problems of easy hygroscopic decomposition, high toxicity, insufficient stability and the like, and achieves low cost, low toxicity and stability high effect
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Embodiment 1
[0049] Embodiment one: the synthesis of benzyl diphenylphosphine oxide
[0050]
[0051] With phenylacetic acid and diphenylphosphine oxide as raw materials, the reaction steps are as follows:
[0052] Add phenylacetic acid (68 mg, 0.5 mmol), diphenylphosphine oxide (101 mg, 0.5 mmol), sodium persulfate (119 mg, 0.5 mmol), silver oxide (6.2 mg, 0.05 mmol) and methanol to a reaction vial / water (2.5 mL: 2.5 mL), room temperature (25 o c) reaction;
[0053] TLC tracking reaction until complete completion;
[0054] The crude product obtained after the reaction was separated by column chromatography (dichloromethane:methanol=95:5) to obtain the target product (yield 84%). The analytical data of the product are as follows: 1 H NMR (400 MHz, DMSO-d 6 ) δ 7.85–7.77 (m, 4H), 7.60–7.44 (m, 6H), 7.28–7.15 (m, 5H), 6.48 (dd, J = 17.8, 5.8 Hz, 1H), 5.62(t, J = 6.4 Hz, 1H).
Embodiment 2
[0055] Example 2: Synthesis of (2-chlorobenzyl)-bis(4-methoxyphenyl)phosphine oxide
[0056] With 2-chlorophenylacetic acid and bis(4-methoxyphenyl)phosphine oxide as raw materials, the reaction steps are as follows:
[0057] Add 2-chlorophenylacetic acid (85 mg, 0.5 mmol), bis(4-methoxyphenyl)phosphine oxide (262 mg, 1 mmol), potassium persulfate (270 mg, 1.0 mmol), carbonic acid Silver (27.5 mg, 0.1 mmol) and ethanol (5 mL), 40 o C reaction;
[0058] TLC tracking reaction until complete completion;
[0059] The crude product obtained after the reaction was separated by column chromatography (dichloromethane:methanol=90:10) to obtain the target product (yield 83%). The analytical data of the product are as follows: 1 H NMR (400 MHz, DMSO-d 6 ) δ 7.89–7.80 (m,4H), 7.64–7.48 (m, 4H), 7.32–7.19 (m, 4H), 6.50 (dd, J = 17.8, 5.8 Hz, 1H), 5.68 (t, J = 6.4 Hz, 1H), 3.67 (s, 6H).
Embodiment 3
[0060] Example 3: Synthesis of (3-chlorobenzyl)-bis(4-tolyl)phosphine oxide
[0061] With 3-chlorophenylacetic acid and two (4-tolyl) phosphine oxide as raw materials, the reaction steps are as follows:
[0062] Add 3-chlorophenylacetic acid (85 mg, 0.5 mmol), bis(4-methylphenyl)phosphine oxide (345 mg, 1.5 mmol), ammonium persulfate (342 mg, 1.5 mmol), silver acetate (25 mg, 0.15 mmol) and acetonitrile, 60 o C reaction;
[0063] TLC tracking reaction until complete completion;
[0064] The crude product obtained after the reaction was separated by column chromatography (dichloromethane:methanol=95:5) to obtain the target product (yield 80%). The analytical data of the product are as follows: 1 H NMR (400 MHz, DMSO-d 6 ) δ 7.88–7.81 (m, 4H), 7.65–7.47 (m, 4H), 7.31–7.18 (m, 4H), 6.51 (dd, J = 17.8, 5.8 Hz, 1H), 5.66(t, J = 6.4 Hz, 1H), 2.21 (s, 6H).
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