反应详情

Into a solution containing 8.2 g (0.02 moles) of tetraisopropyl (dichloromethylene)bisphosphonate in 70 ml of ethanol, 9.0 g of sodium sulphite in 250 ml of water are added while stirring during 15 minutes at 10° to 15° C., whereafter the mixture is stirred for 1 h. The mixture is extracted with chloroform and the extract is dried (MgSO4) and filtered. The filtrate is evaporated under a vacuum, whereby about 7.6 g (100% of the theor.) of tetraisopropyl (monochloromethylene)bisphosphonate (31P-NMR (CDCl3 : δ 12.04 ppm) are obtained as a colourless oil, at a concentration of 98%.

1. additionare added
2. stirringis stirred for 1 h
3. extractionThe mixture is extracted with chloroform
4. dry with materialthe extract is dried (MgSO4)
5. filtrationfiltered
6. customThe filtrate is evaporated under a vacuum, whereby about 7.6 g (100% of the theor