Ethyl 3-amino-2-methylpropyl(diethoxymethyl)phosphinate → 3-Amino-2-methylpropylphosphonous acid monohydrate

A solution of 6.0 g of ethyl 3-amino-2-methylpropyl(diethoxymethyl)phosphinate in 30 ml of 36% aqueous hydrochloric acid is heated to reflux for a period of 7 hours. The reaction mixture is then allowed to cool to room temperature, concentrated under reduced pressure and co-evaporated twice with 10 ml of water under reduced pressure. The crude product is dissolved in 50 ml of dry ethanol and 5 ml of propylene oxide is added dropwise. The precipitated solid is collected by filtration and dried to give 3-amino-2-methylpropyl-phosphonous acid monohydrate, m.p. 96°-100° C., 31P=+25.8 ppm (D2O).

1. temperatureto reflux for a period of 7 hours
2. concentrationconcentrated under reduced pressure
3. dissolutionThe crude product is dissolved in 50 ml of dry ethanol
4. addition5 ml of propylene oxide is added dropwise
5. filtrationThe precipitated solid is collected by filtration
6. customdried

ORDレコード

ord-5e929b07e6b94d928d7c01f83081b6a3

出典データセット

uspto-grants-1991_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05004826