Benzoxazole derivative and preparation method and application thereof
A technology for benzoxazole derivatives, applied in the field of benzoxazole derivatives and their preparation, can solve the problems of poor solubility, difficult synthesis and purification, and low oral bioavailability, and achieve good anti-inflammatory activity and good The effect of inhibiting activity
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[0050] The present invention also provides a preparation method of a benzoxazole derivative having a structure shown in formula (I), comprising:
[0051] The compound of formula (II) structure and the compound of formula (III) structure are reacted, obtain the compound of formula (I) structure;
[0052]
[0053] where the R 1 hydrogen, C1-C15 alkyl, halogen, C1-C15 alkoxy, nitro, cyano, C3-C8 cycloalkyl, C2-C12 heterocyclyl, -COR 2 、-COOR 2 、-SO 2 R 2 or -NR 3 R 4 ;
[0054] The R 2 , R 3 , R 4 Independently selected from hydrogen or C1~C10 alkyl;
[0055] Said n is 1, 2, 3 or 4;
[0056] said C3-C7 cycloalkyl, C2-C7 heterocyclyl, substituted C6-C20 aryl, unsubstituted C6-C20 aryl, unsubstituted C5-C20 heteroaryl or substituted C5-C20 C20 heteroaryl.
[0057] In the present invention, the present invention has no special requirements for the reaction method of the compound of the formula (II) structure and the compound of the formula (III) structure to obtain...
Embodiment 1
[0063]
[0064] Synthesis of 2-chloromethylbenzoxazole:
[0065] Add 2-aminophenol (1.635g), 1.2ml of chloroacetyl chloride, 0.5ml of pyridine, and 20ml of chlorobenzene into a 50ml round-bottomed flask, stir at room temperature for 2h, add 0.258g of p-toluenesulfonic acid, reflux for 6h, and monitor with TCL. After the reaction, chlorobenzene was evaporated, 100ml of water was added, extracted with ethyl acetate, 20ml*3, dried with anhydrous magnesium sulfate and then rotary evaporated. The product was passed through the column with DCM to obtain a yellow oily liquid as the product.
[0066] 1 H NMR (600MHz, CDCl 3 )δ7.73-7.70 (m, 1H), 7.53-7.51 (m, 1H), 7.38-7.32 (m, 2H), 4.73 (s, 2H)
Embodiment 2
[0068]
[0069] Synthesis of N-(Benzo[d]oxazol-2-ylmethyl)aniline
[0070]Put 2-chloromethylbenzoxazole, aniline, KI, K2CO3 into 10ml DMF at a molar ratio of 1:1:0.15:1, heat to reflux at 55°C, monitor the reaction by TLC, and the reaction is complete after about 6 hours. Extraction, drying, PE: DCM = 7: 1 column, a white solid was obtained with a yield of 82%.
[0071] 1 H NMR (600MHz, CDCl3) δ7.71-7.69 (m, 1H), 7.51-7.48 (m, 1H), 7.33-7.30 (m, 2H), 7.20 (dd, J=11.8, 4.1Hz, 2H), 6.79-6.74(m, 3H), 4.61(s, 2H).
[0072] 13 C NMR (151MHz, CDCl 3 )δ164.08, 150.85, 146.84, 140.86, 129.35, 129.25, 125.05, 124.43, 119.95, 118.61, 115.12, 113.21, 110.63, 77.21, 77.00, 76.79, 41.92.
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