反应详情

温度

80 °C

A solution of 7-bromo-1,1-dimethyl-1,2,3,4-tetrahydro-naphthalene (Compound 15, 1.20 g, 5.94 mmol) in 20 ml of THF was first degassed by bubbling with argon for 30 min. Tributyl(1-ethoxyvinyl)tin (4.29 g, 11.88 mmol) and PdCl2(PPh3)2 (422 mg, 0.60 mmol) were added. After stirring at 80° C. for 18 h, the mixture was cooled to room temperature and 3 mL of 10 % HCl was added. The mixture was then stirred for another 30 min, then extracted with ethyl acetate (3×10 mL). The combined organic layer was washed with brine (1×10 mL), dried (MgSO4) and concentrated at reduced pressure. Purification by flash chromatography (80:20 hexane/ethyl acetate) afforded the title compound (669 mg, 56% yield) as a colorless oil:

1. customby bubbling with argon for 30 min
2. temperaturethe mixture was cooled to room temperature
3. stirringThe mixture was then stirred for another 30 min
4. extractionextracted with ethyl acetate (3×10 mL)
5. washThe combined organic layer was washed with brine (1×10 mL)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated at reduced pressure
8. customPurification by flash chromatography (80:20 hexane/ethyl acetate)