A compound and its preparation method and application
A kind of technology of compound and pharmaceutical preparation, applied in the field of compound and preparation thereof
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Embodiment 1
[0049] Example 1: Preparation of 4-((3,5,6-trimethylpyrazin-2-yl)methoxy)benzyl alcohol
[0050] a. Preparation of intermediate 2-hydroxymethyl-3,5,6-trimethylpyrazine
[0051] The reference (Liu Xinyong. Synthesis of Ligustrazine metabolites in vivo. Journal of Shandong Medical University. 1997, 35(1)) method can easily prepare the compound 2-hydroxymethyl-3,5,6-trimethylpyrazine . The synthetic route is shown in the figure below:
[0052]
[0053] The product is a yellow solid, 1 H-NMR (500MHz, CDCl 3 , δppm): δ4.66 (s, 2H), δ4.31 (s, 1H), δ2.50 (s, 6H), δ2.38 (s, 3H).
[0054] b. Preparation of intermediate 4-((3,5,6-trimethylpyrazin-2-yl)methoxy)benzaldehyde
[0055] In the reaction flask, add 2-hydroxymethyl-3,5,6-trimethylpyrazine (3g, 0.02mol), dissolve in 20mL dichloromethane, add thionyl chloride (3mL, 0.04mol), stirred for 1.5h. After TLC monitors that the reaction is complete, evaporate the solvent and the remaining thionyl chloride to dryness under reduce...
Embodiment 2
[0059] Example 2: Preparation of 4-(3,5,6-trimethylpyrazine-2-yloxy)benzyl alcohol
[0060] a. Preparation of intermediate 2-carboxy-3,5,6-trimethylpyrazine
[0061] The reference (Liu Xinyong. Synthesis of metabolites of ligustrazine in vivo. Journal of Shandong Medical University. 1997, 35 (1)) method, the compound 2-carboxy-3,5,6-trimethylpyrazine can be easily prepared. The synthetic route is shown in the figure below:
[0062]
[0063] The product is a white solid, 1 H-NMR (500MHz, CDCl 3 , δppm): δ10.18 (s, 1H), δ2.89 (s, 3H), δ2.61 (s, 3H), δ2.56 (s, 3H).
[0064] b. Preparation of intermediate 4-(3,5,6-trimethylpyrazine-2-yloxy)benzaldehyde
[0065] In the reaction flask, add 3,5,6-trimethylpyrazine-2-carboxylic acid (13.8g, 0.08mol), DCC (dicyclohexylcarbodiimide, 26g, 0.126mol), DMAP (4-dimethyl Aminopyridine, 0.5g, 0.004mol), p-Hydroxybenzaldehyde (8g, 0.06mol), 100mL of dichloromethane, stirred at room temperature for 24h, after the reaction was complete as...
Embodiment 3
[0068] Example 3: Preparation of 4-nicotinoyloxybenzyl alcohol
[0069] a. Preparation of intermediate 4-nicotinyloxybenzaldehyde
[0070] In the reaction bottle, add nicotinic acid (2.5g, 0.02mol), 20mL of acetone, dropwise add thionyl chloride (4mL, 0.05mol) under ice bath stirring, heat and reflux for 2 hours, evaporate the solvent and oxychloride under reduced pressure Sulfone to obtain 2.7g of nicotinoyl chloride, add 20mL of acetone for later use.
[0071] In another reaction flask, add p-hydroxybenzaldehyde (2.4g, 0.02mol), 20mL acetone, triethylamine (3mL, 0.02mol), and add the above-prepared nicotinoyl chloride (2.7g, 0.02mol) dropwise under stirring in an ice bath ) in acetone solution. The mixture was heated to 60° C. and reacted for 2 h. After the reaction was completed as monitored by TLC, the reaction solution was cooled to room temperature, filtered, and the filter cake was washed three times with acetone. The filtrate was concentrated under reduced pressure ...
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