Methanol → Diethyl 3-(N-Hydroxyamino)propylphosphate

To a solution of hydroxylamine hydrochloride (55.6 g.) in water (100 ml.) were added solution of sodium hydroxide (32.0 g.) in water (75 ml.) under ice-cooling and then methanol (75 ml.). To this solution was added dropwise diethyl 3-bromopropylphosphonate (25.5 g.), whereafter the mixture was warmed at 40°-45° C. for 3 hours with stirring. The methanol was distilled off under reduced pressure. The resultant aqueous solution was adjusted to pH 8 with sodium bicarbonate, washed three times with benzene which were discarded (once with 150 ml. and twice with 100 ml. portions) and then extracted with three 150 ml. portions of chloroform. The chloroform extracts were combined, dried over magnesium sulfate and evaporated to dryness under reduced pressure to give oily diethyl 3-(N-hydroxyamino)propylphosphonate (13.05 g.).

1. temperaturecooling
2. temperaturewhereafter the mixture was warmed at 40°-45° C. for 3 hours
3. distillationThe methanol was distilled off under reduced pressure
4. washwashed three times with benzene which
5. extractionportions) and then extracted with three 150 ml
6. dry with materialdried over magnesium sulfate
7. customevaporated to dryness under reduced pressure

ORDレコード

ord-ff541e99301d4597abde208ba037a349

出典データセット

uspto-grants-1980_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04206156