Hydrochloric Acid → HCID 85631143, compound

HRID 1463630Notes

Reaction equation

HRID 1463630 reaction equation
C1(=O)[N:5]([CH2:6][CH:7]([O:18][Si](C)(C)C)[CH2:8][P:9]([CH2:14][CH2:15][CH2:16][CH3:17])(=[O:13])[O:10]CC)C(=O)C2=CC=CC=C12.[ClH:29]>>[ClH:29].[NH2:5][CH2:6][CH:7]([OH:18])[CH2:8][P:9]([CH2:14][CH2:15][CH2:16][CH3:17])(=[O:10])[OH:13]

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 10093926HCID 10093926, compound

Product 1

HCID 85631143HCID 85631143, compound

Procedure

The solution of 2.4 g of ethyl 3-phthalimido-2-trimethylsiloxy-propyl(n-butyl)phosphinate in 50 ml of concentrated aqueous hydrochloric acid is heated to reflux for 20 hours. After this time the suspension is cooled to room temperature and filtered. The filtrate is evaporated to dryness and the resulting semi-solid is co-evaporated with water (5×50 ml) and absolute ethanol (5×100 ml) and the white solid dried in high vacuum overnight. Crystallisation from absolute ethanol affords 3-amino-2-hydroxy-propyl(n-butyl)phosphinic acid hydrochloride, m.p. 158°-160°.

Workup

  1. temperatureto reflux for 20 hours
  2. filtrationfiltered
  3. customThe filtrate is evaporated to dryness
  4. customthe white solid dried in high vacuum overnight
  5. customCrystallisation from absolute ethanol

Sources & evidence

ORD record
ord-cb8fb5f42db44ec18f0ebaaafb3719ee
Source dataset
uspto-grants-1994_04
Patent number
US05300679

Reaction notes

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