The preparation method of 2-substituted benzoxazole compounds
A technology for benzoxazole and compounds, which is applied in the field of preparation of 2-substituent benzoxazole compounds, can solve the problem of unsuitable large-scale safe production of 2-substituent benzoxazole compounds and the harsh conditions of the preparation process , unstable reactants, etc.
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Embodiment 1
[0022] Example 1: Preparation of 2-Phenylbenzoxazole
[0023]
[0024] (1) Synthesis of substrate: Take 3.6mmol of o-nitrophenol into the flask, add 1mL of pyridine, and mix well to obtain a dark brown liquid. 3.9 mmol of benzoyl chloride was added to obtain a pale yellow milky substance, which was stirred magnetically for 4 h at room temperature. The product was extracted (water was added to quench the reaction, saturated sodium chloride was added to prevent emulsification), the organic phase was obtained by standing at room temperature, and the organic phase was dried at room temperature for 1 hour. The resulting dried product is separated by column chromatography, and the eluted product is spin-dried using a rotary evaporator to obtain the reaction raw material.
[0025] (2) Synthesis of 2-phenylbenzoxazole: Take 1.0 mmol substrate and put it in a flask, add 4.0 mmol ammonium formate, 20 mL glacial acetic acid, and finally add 5% palladium-carbon with 10% raw material content. ...
Embodiment 2
[0026] Example 2: Preparation of 5-methyl-2-benzoxazole
[0027]
[0028] (1) Synthesis of reaction substrate: Take 3.6 mmol 4-methyl-2-nitrophenol into a flask, add 1 mL pyridine, and mix uniformly to obtain a dark brown liquid. Add 3.9 mmol of benzoyl chloride to obtain a pale yellow milky substance, which was stirred magnetically for 4 hours at room temperature. The product was extracted (water was added to quench the reaction, saturated sodium chloride was added to prevent emulsification), the organic phase was obtained by standing at room temperature, and the organic phase was dried at room temperature for 1 hour. The obtained dried product and the obtained dried product are separated by column chromatography, and the eluted product is spin-dried using a rotary evaporator to obtain the reaction raw material.
[0029] (2) Preparation of the target compound: take 1.0 mmol substrate into a flask, add 4.0 mmol ammonium formate, 20 mL glacial acetic acid, and finally add 10% of th...
Embodiment 3
[0030] Example 3: 5-tert-butyl-2-benzoxazole
[0031]
[0032] (1) Synthesis of reaction substrate: Take 3.6 mmol of 4-tert-butyl-2-nitrophenol into a flask, add 1 mL of pyridine, and mix uniformly to obtain a dark brown liquid. Add 3.9 mmol of benzoyl chloride to obtain a pale yellow milky substance, which was stirred magnetically for 4 hours at room temperature. The product was extracted (water was added to quench the reaction, saturated sodium chloride was added to prevent emulsification), the organic phase was obtained by standing at room temperature, and the organic phase was dried at room temperature for 1 hour. The resulting dried product is separated by column chromatography, and the eluted product is spin-dried using a rotary evaporator to obtain the reaction raw material.
[0033] (2) Preparation of the target compound: take 1.0 mmol substrate into a flask, add 4.0 mmol ammonium formate, 20 mL glacial acetic acid, and finally add 10% of the raw material content of the ca...
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