反应详情

Tetramethylguanidine (42.3 g; 0.37 mole) was slowly added to a solution of 4-benzyloxybenzaldehyde (75.6 g; 0.36 mole) and (1,2-diethoxy-2-oxoethyl) (triphenyl)phosphonium chloride (130.7 g; 0.304 mole) dissolved in chloroform (800 ml) at 0° C. After stirring at room temperature over night, the solvent was evaporated in vacuo. The residue was dissolved in diethyl ether, insoluble material was filtered off and the filtrate was washed with sodium bicarbonate and dried (magnesium sulfate). The procedure was repeated once and thereafter the crude product was stirred overnight with a sodium bisulfite saturated water solution. The solid material was filtered off, the product was extracted with diethyl ether, dried (magnesium sulfate) and the solvent was evaporated in vacuo to give 85 g (yield 73%) of the desired product.

1. customthe solvent was evaporated in vacuo
2. dissolutionThe residue was dissolved in diethyl ether
3. filtrationinsoluble material was filtered off
4. washthe filtrate was washed with sodium bicarbonate
5. dry with materialdried (magnesium sulfate)
6. stirringthe crude product was stirred overnight with a sodium bisulfite saturated water solution
7. filtrationThe solid material was filtered off
8. extractionthe product was extracted with diethyl ether
9. dry with materialdried (magnesium sulfate)
10. customthe solvent was evaporated in vacuo