反应详情

Methyl lithium (1.5M, 96 ml) was added dropwise to a solution of 4,5,6,7-tetrahydro-1-methyl-indan-3-one (17.7 g, 0.118 mol) in 50 ml of diethyl ether under an argon atmosphere whereupon the reaction mixture was refluxed for 18 hours. The mixture after this time period was hydrolyzed and the reaction mixture extracted with diethyl ether. The ether extracts were dried over anhydrous MgSO4 and filtered. To the ether solution, 0.5 ml of 6M HCl was added and the solution stirred for one hour. After this time period the ether solution was washed with water, dried over anhydrous MgSO4, filtered and concentrated. Distillation at reduced pressure afforded 8.0 g (45 percent) of product.

1. temperaturewas refluxed for 18 hours
2. extractionthe reaction mixture extracted with diethyl ether
3. dry with materialThe ether extracts were dried over anhydrous MgSO4
4. filtrationfiltered
5. additionTo the ether solution, 0.5 ml of 6M HCl was added
6. washAfter this time period the ether solution was washed with water
7. dry with materialdried over anhydrous MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. distillationDistillation at reduced pressure