反应详情

To a suspension of 3.6 g (10.1 mmol) of methyltriphenylphosphonium bromide in 50 mL tetrahydrofuran under nitrogen at -50° C. is added n-butyllithium (10 mm as a hexane solution (2.1 M)). After 45 minutes, a solution of 3.0 g (9.90 mmol) of 3,4-dihydro-7-(2-quinolinylmethoxy)-1(2H)-naphthalenone, prepared according to Example 1A above, in 50 mL tetrahydrofuran is added dropwise and the reaction mixture is allowed to slowly come to room temperature. After three days, 50 mL water and 50 mL ether is added. The organic layer is separated, dried over magnesium sulfate and evaporated to 5.0 g of crude product. Chromatography accords 1.3 g (44%) of the desired product. Recrystallization from hexane gives 0.70 g (24%) of white crystals mp 56°-58° C.

1. additionis added dropwise
2. customto slowly come to room temperature
3. waitAfter three days
4. customThe organic layer is separated
5. dry with materialdried over magnesium sulfate
6. customevaporated to 5.0 g of crude product
7. customRecrystallization from hexane