Carbon Dioxide → HCID 13633544, compound

Participants

Reaction Conditions

Reaction Steps

The product obtained in Example 3 (2.1 g), dimethylaminopyridine (150 mg) and triethylamine (10 cc) are introduced, under an argon atmosphere, into a three-neck flask and acetic anhydride (6 cc) is then added rapidly, with stirring, at a temperature of 25° C. After 1 hour's stirring, water (20 cc) is added and the reaction mixture is thereafter neutralised by gradual addition of sodium carbonate until the evolution of carbon dioxide gas ceases. The reaction mixture is extracted with ethyl acetate (twice 50 cc). The organic phase is washed with a 0.1N aqueous hydrochloric acid solution (3 times 50 cc). The organic phases are dried over magnesium sulphate. After filtration and evaporation of the solvent, the residue obtained is taken up in hexane. The precipitate which forms is filtered off. This gives a 93% yield of 2,5,7,8-tetramethyl-2-(4',8',12'-trichloro-4',8',12'-trimethyl-tridecyl)-chroman-6-ol acetate, melting at 95°-105° C.

Provenance & Evidence