N-substituted-2-(2-hydroxybenzyl) glycine amide compound and preparing method and application thereof
A technology of aminoacetamide and hydroxybenzyl, applied in the field of pesticides
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Embodiment 1
[0041] Example 1: Synthesis of N-benzyl-2-(2-hydroxybenzyl)aminoacetamide.
[0042] In a 150 mL round bottom flask with reflux condenser and desiccator, add 4.560 g (20 mmol) of N-benzyl-2-bromoacetamide, 2.953 g (24 mmol) of 2-(aminomethyl)phenol, and anhydrous carbonic acid Potassium 3.312g (24mmol), 50mL DMF and THF mixed solvent (V:V=1:1), heated to 65°C and stirred for 3h, followed by TLC plate detection. After the reaction, the solvent was removed under reduced pressure, 40 mL of water was added, and extraction was performed with ethyl acetate (50 mL×3 times). The organic layers were combined and washed with water (40 mL×2 times) and saturated brine (40 mL×2 times) in turn. Drying with anhydrous sodium sulfate, filtering with suction, and concentrating under reduced pressure to obtain a crude product, which is separated by column chromatography to obtain a white solid; mp 107.6-108.4°C, yield 68.7%.
[0043] 1 HNMR(500MHz, CDCl 3 )δ: 7.33-7.30 (m, 2H), 7.25-7.22 (m, 2H), 7.1...
Embodiment 2
[0046] Example 2: Synthesis of N-(2-methylbenzyl)-2-(2-hydroxybenzyl)aminoacetamide.
[0047] In a 150 mL round bottom flask with reflux condenser and desiccator, 4.840 g (20 mmol) of N-(2-methylbenzyl)-2-bromoacetamide and 2.953 g of 2-(aminomethyl)phenol were added. 24mmol), 3.312g (24mmol) of anhydrous potassium carbonate, 50mL of a mixed solvent of DMF and THF (V:V=1:1), heated to 65°C and stirred for 3h, followed by TLC plate detection. After the reaction, the solvent was removed under reduced pressure, 40 mL of water was added, and extraction was performed with ethyl acetate (50 mL×3 times). The organic layers were combined and washed with water (40 mL×2 times) and saturated brine (40 mL×2 times) in turn. Drying with anhydrous sodium sulfate, filtering with suction, and concentrating under reduced pressure to obtain a crude product, which is separated by column chromatography to obtain a white solid; mp 142.2-143.8°C, yield 64.4%.
[0048] 1 HNMR(500MHz, CDCl 3 )δ:7.11(t,J=7...
Embodiment 3
[0051] Example 3: Synthesis of N-(4-methylbenzyl)-2-(2-hydroxybenzyl)aminoacetamide.
[0052] In a 150 mL round bottom flask with reflux condenser and desiccator, 4.840 g (20 mmol) of N-(4-methylbenzyl)-2-bromoacetamide and 2.953 g of 2-(aminomethyl)phenol were added. 24mmol), 3.312g (24mmol) of anhydrous potassium carbonate, 50mL of a mixed solvent of DMF and THF (V:V=1:1), heated to 65°C and stirred for 3h, followed by TLC plate detection. After the reaction, the solvent was removed under reduced pressure, 40 mL of water was added, and extraction was performed with ethyl acetate (50 mL×3 times). The organic layers were combined and washed with water (40 mL×2 times) and saturated brine (40 mL×2 times) in turn. Drying with anhydrous sodium sulfate, filtering with suction, and concentrating under reduced pressure to obtain a crude product, which is separated by column chromatography to obtain a white solid; mp 122.6-123.5°C, yield 67.2%.
[0053] 1 HNMR(500MHz, CDCl 3 )δ: 7.28 (s, ...
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