반응 #5263

반응 방정식

ethyl 3-amino-2-methylpropyl(diethoxymethyl)phosphinate

→

3-amino-2-methylpropyl-phosphonous acid monohydrate

용매

hydrochloric acid

반응 조건

후처리

1. 1
   온도to reflux for a period of 7 hours
2. 2
   농축concentrated under reduced pressure
3. 3
   workup.DISSOLUTIONThe crude product is dissolved in 50 ml of dry ethanol
4. 4
   workup.ADDITION5 ml of propylene oxide is added dropwise
5. 5
   여과The precipitated solid is collected by filtration
6. 6
   기타dried

실험 절차

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).

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