反应详情

A solution of 4 g (16 mmol) of 5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene-2-carbonyl chloride and 4 g (16 mmol) of methyl 4-bromomethylbenzoate in 20 ml of dimethoxyethane was added dropwise to a solution or suspension of 0.56 g of bis(triphenylphosphine)palladium(II) dichloride and 2.1 g of zinc powder in 40 ml of dimethoxyethane at room temperature. The reaction mixture was then refluxed for 6 h. After cooling, solids were filtered off and the filtrate was heated with active carbon and filtered hot. The filtrate was concentrated and yielded after recrystallization 3× from methanol and finally from isopropanol 0.9 g of the title compound of melting point 103°-104° C.

1. temperatureThe reaction mixture was then refluxed for 6 h
2. temperatureAfter cooling
3. filtrationsolids were filtered off
4. temperaturethe filtrate was heated with active carbon
5. filtrationfiltered hot
6. concentrationThe filtrate was concentrated
7. customyielded
8. customafter recrystallization 3× from methanol