反应详情

A mixture of 1.0 g of ethyl 3-oxobutyl(diethoxymethyl)phosphinate 2.85 g of ammonium acetate and 0.16 g of sodium cyanoborohydride in 20 ml of methanol is stirred for 2.5 hours. After standing overnight, the pH is adjusted to pH 5,6 with 2 N hydrochloric acid. The mixture is then evaporated to dryness. 20 ml of water are added and the mixture is washed 3 times with 20 ml of diethyl ether. The aqueous layer is adjusted to pH 12 with potassium hydroxide and extracted 4 times with 25 ml of chloroform. The organic layers are combined, dried, filtered and evaporated to dryness yielding ethyl 3-aminobutyl(diethoxymethyl)phosphinate, 31P-NMR spectrum: δ=±46.0 ppm (CDCl3).

1. waitAfter standing overnight
2. customThe mixture is then evaporated to dryness
3. addition20 ml of water are added
4. washthe mixture is washed 3 times with 20 ml of diethyl ether
5. extractionextracted 4 times with 25 ml of chloroform
6. customdried
7. filtrationfiltered
8. customevaporated to dryness