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ChemicalBook CAS DataBase List Arbidol
131707-25-0

Arbidol synthesis

9synthesis methods
-

Yield:131707-25-0 60%

Reaction Conditions:

Stage #1: formaldehyd;dimethyl aminewith acetic acid in water at 0; for 0.25 h;
Stage #2: 6-bromo-5-hydroxy-1-methyl-2-phenylthiomethylindole-3-carboxylic acid ethyl ester in water at 80; for 4 h;

Steps:

4 Example 4

Set up the device, add 100mL glacial acetic acid solution to the three-necked flask, cool to 0, slowly add 40mL 40% methylamine aqueous solution, then add 10mL 37% formaldehyde aqueous solution, after stirring the reaction for 15 min, add 6 Bromo-5-hydroxy-1-methyl-2-phenylthiomethylindole-3-carboxylic acid ethyl ester (12.6g, 0.03moL), stir well for 10 minutes, then start to heat up to 80, maintain the reaction temperature After completely dissolved, react for 4 hours. After the reaction is over, pour the reaction solution into water, add an appropriate amount of 20% potassium hydroxide solution to neutralize with stirring, adjust the pH of the solution to 7.0, precipitate solids, filter with suction, and wash once with water. The solid was obtained by suction filtration, and dried in an oven at 70°C for 5 hours to obtain a crude product. Recrystallize with acetonitrile. After it is completely dissolved, add 1g of activated carbon to reflux for 30 min, filter it hot, and cool it, and 8.5 g of brown solid Arbidol is precipitated. 60% yield

References:

CN111533677,2020,A Location in patent:Paragraph 0015

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