Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List Vanillin acetate
881-68-5

Vanillin acetate synthesis

11synthesis methods
By acetylation of vanillin or by oxidation of isoeugenyl acetate with chromic acid in the presence of sulfanilic acid; also by electrolytic reduction of vanillin, followed by acetylation of vanillyl alcohol.
-

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

Vanillin acetate Related Search: