Ammonia → Hydrochloric Acid

A mixture of diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-methylpropylphosphonate (28.3 g.). and conc. hydrochloric acid (280 ml.) was refluxed for 18 hours and then concentrated under reduced pressure to give an oily residue. To the residue was added a mixture of water (100 ml.) and ethyl acetate (100 ml.). From the resultant mixture, the aqueous layer was separated, treated with activated charcoal and concentrated under reduced pressure to give an oily residue. The residue was dissolved in a mixture of methanol (30 ml.) and water (15 ml.). The solution was adjusted to pH 4.0 with aqueous ammonia under ice-cooling and concentrated under reduced pressure to give a residue, which was passed through a column of anion exchange resin, Amberlite IRA-400 (OH- form). The column was washed with water and then the object compound was eluted with 1 N hydrochloric acid. The eluate was concentrated under reduced pressure to give oily hydrochloric acid salt of 3-(N-hydroxyamino)-2-methylpropylphosphonic acid (9.6 g.).

1. concentrationconcentrated under reduced pressure
2. customto give an oily residue
3. additionTo the residue was added
4. customFrom the resultant mixture, the aqueous layer was separated
5. additiontreated with activated charcoal
6. concentrationconcentrated under reduced pressure
7. customto give an oily residue
8. temperaturecooling
9. concentrationconcentrated under reduced pressure
10. customto give a residue, which
11. washThe column was washed with water
12. washthe object compound was eluted with 1 N hydrochloric acid
13. concentrationThe eluate was concentrated under reduced pressure

ORD 기록

ord-4a7d27288e53415ca6e4f1101c5d20f5

출처 데이터셋

uspto-grants-1980_01

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04182758