反应详情

3.1 g (12 mmol) of 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthylglyoxylic acid and 50 ml of THF are introduced into a three-necked flask. At 0° C. and under a stream of nitrogen, 16 ml (48 mmol) of a solution of ethylmagnesium iodide in ethyl ether (3M) are added dropwise and the mixture is stirred at room temperature for four hours. The reaction medium is poured into water, the mixture is extracted with ethyl ether and the organic phase is separated after settling has taken place, then dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a silica column and eluted with a mixture of dichloromethane and ethyl ether (20:80). After evaporation of the solvents, 2.6 g (79%) of the expected product, melting point 168°-169° C., are collected.

1. extractionthe mixture is extracted with ethyl ether
2. customthe organic phase is separated after settling
3. dry with materialdried over magnesium sulphate
4. customevaporated
5. customThe residue obtained
6. customis purified by chromatography on a silica column
7. washeluted with a mixture of dichloromethane and ethyl ether (20:80)
8. customAfter evaporation of the solvents, 2.6 g (79%) of the expected product, melting point 168°-169° C.
9. customare collected