A kind of process method for preparing 5-bromoisochroman-4-one without catalyst method
A process method, the technology of isochroman, which is applied in the field of preparation of chemical raw materials, can solve the problems of high production cost of isochroman-4-one, unfavorable large-scale production and use, and difficulty in purification of finished compounds, so as to reduce production cost, Reduced production costs and cheap raw materials
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Embodiment 1
[0026] Take 2 mL of cyclohexane, 0.5 mmol of 5-bromoisochroman, and a magnetron into a high-pressure reactor with a polytetrafluoroethylene liner, and then pass oxygen into the reactor until the pressure of the oxygen in the reactor is Then, seal the reaction kettle, put it into a heating tank with a temperature of 140° C., and carry out the reaction for 20 h under the condition of magnetic stirring. After the reaction was completed, the reaction system was cooled to room temperature, and then, the internal standard quantitative analysis of the obtained product was carried out using a gas chromatograph, and the yield of 5-bromoisochroman-4-one was measured to be 87%. Afterwards, the product is separated and purified by column chromatography to obtain the finished product of 5-bromoisochroman-4-one. use 1 H-NMR, 13 C-NMR confirms the structure of the product in the appendix figure 1 And attached figure 2 .
Embodiment 2
[0028] Take 2 mL of n-hexane, 0.5 mmol of 5-bromoisochroman, and magnetons into a high-pressure reactor with a polytetrafluoroethylene liner, and then pass oxygen into the reactor until the pressure of oxygen in the reactor is 0.5 MPa, then, seal the reaction kettle, put it into a heating tank with a temperature of 140° C., and carry out the reaction for 20 h under the condition of magnetic stirring. After the reaction was completed, the reaction system was cooled to room temperature, and then, the internal standard quantitative analysis of the obtained product was carried out using a gas chromatograph, and the yield of 5-bromoisochroman-4-one was measured to be 82%. Afterwards, the product is separated and purified by column chromatography to obtain the finished product of 5-bromoisochroman-4-one.
Embodiment 3-8
[0030] Change the oxygen pressure in Example 2 to 0.2MPa, 0.7MPa, 1MPa, 1.5MPa, 2MPa, 3MPa, and other conditions remain unchanged to obtain the productive rate of 5-bromoisochroman-4-one product (gas phase internal standard) They were 43%, 81%, 65%, 61%, 67%, and 49%, respectively.
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