反应详情

温度

0 °C

1 g of 7,7-dimethyloctanoic acid is dissolved in 20 ml of DCM cooled to 0° C., 0.57 ml of oxalyl chloride is added and the mixture is then left stirring for 1 hour at 0° C. and for 2 hours at RT. 0.93 ml of 2,5-dimethoxytoluene and one drop of DMF are added, the mixture is cooled to 0° C., 940 mg of AlCl3 are then added and the mixture is left stirring for 1 hour at 0° C. and overnight at RT. It is poured into 10% HCl solution and extracted with ether, and the combined organic phases are then washed with 2N sodium hydroxide, dried and concentrated. The residue is chromatographed on silica, eluting with DCM/pentane (85/15; v/v) to give 1.05 g of the expected compound.

1. waitthe mixture is then left
2. temperaturethe mixture is cooled to 0° C.
3. waitthe mixture is left
4. stirringstirring for 1 hour at 0° C. and overnight at RT
5. extractionextracted with ether
6. washthe combined organic phases are then washed with 2N sodium hydroxide
7. customdried
8. concentrationconcentrated
9. customThe residue is chromatographed on silica
10. washeluting with DCM/pentane (85/15; v/v)