反应详情

In a stream of argon, to 25 ml of tetrahydrofuran was added 3.3 g of phenyllithium (19% solution in dibutylether) (7.46 mmol), and 2.68 g (6.79 mmol) of 2-thenyl triphenylphosphonium chloride was added thereto under ice cooling. Next, 2.3 g (6.78 mmol) of 2-benzyloxy-4-dibutylaminobenzaldehyde was dissolved in tetrahydrofuran and added dropwise. The mixture was stirred under ice cooling for 2 hours. After the reaction mixture was poured into water, extraction with ethyl acetate, washing with a saturated saline solution, drying over anhydrous sodium sulfate, and concentration were performed. To the residue, 40 ml of ethyl acetate/hexane (4/1) was added and the precipitate was filtered off. The filtrate was concentrated and then purified by silica gel column chromatography to give 2.64 g of a yellow oily matter (yield: 92.9%).

1. additionwas added
2. additionadded dropwise
3. washwashing with a saturated saline solution
4. dry with materialdrying over anhydrous sodium sulfate, and concentration
5. additionTo the residue, 40 ml of ethyl acetate/hexane (4/1) was added
6. filtrationthe precipitate was filtered off
7. concentrationThe filtrate was concentrated
8. custompurified by silica gel column chromatography
9. customto give 2.64 g of a yellow oily matter (yield: 92.9%)