Vanillin acetate synthesis
- Product Name:Vanillin acetate
- CAS Number:881-68-5
- Molecular formula:C10H10O4
- Molecular Weight:194.18
Yield:881-68-5 120 mg
Reaction Conditions:
with pyridine;dicyclohexyl-carbodiimide in tetrahydrofuran at 0; for 10 h;
Steps:
2 Example 2
Aspirin 0.5g,Vanillin 0.43g,0.22 mL of pyridine dissolved in 2.8 mL of pre-cooled tetrahydrofuran (THF) at 0 ° C,And transferred to a three-necked flask,It was then placed on a magnetic stirrer and stirred in an ice bath.In addition, 0.63 g of dicyclohexylcarbodiimide (DCC) was added to 0.93 mL of 0 ° C pre-cooled THF, and then transferred to a three-necked flask to start the reaction. The temperature of the system was maintained at 0 ° C, stirring was continued for 10 h, and the reaction was monitored by TLC. The reaction is completed and the reaction is stopped. The reaction solution was suction-filtered under reduced pressure, and then filtered to remove white insoluble material (D. Finally, the filtrate was concentrated to dryness under reduced pressure to give a pale yellow crude.The mobile phase was screened by TLC and the separated mobile phase was determined to be petroleum ether-ethyl acetate.50 g of 200-300 mesh column chromatography silica gel was weighed and packed in a petroleum ether wet column. Subsequent preparation of the aspirin derivativeThe crude product was dissolved in ethanol and ethyl acetate, and then mixed with a small amount of silica gel for dry loading. Petroleum ether: ethyl acetate (V:V=30:1) For flow equalization elution, collect and number using tubes, TLC monitor product purity, combine target tubes, decompressConcentrate to dryness and weigh. Acetyl vanillin, white crystals (120 mg);
References:
CN108484397,2018,A Location in patent:Paragraph 0023; 0024; 0025