HCID 67152966, compound → HCID 22717893, compound

HRID 2368206Notes

Reaction equation

HRID 2368206 reaction equation
C([NH:14][P:15]([CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)(=[O:17])[OH:16])(C1C=CC=CC=1)C1C=CC=CC=1>Cl>[NH2:14][P:15]([CH2:18][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)(=[O:16])[OH:17]

Participants

3

Reactant 1

HCID 67152966HCID 67152966, compound

Product 1

HCID 22717893HCID 22717893, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Conditions

Temperature
0 °C

Procedure

A mixture of 20 g of the compound from step 1 and 160 ml of 6N HCl is boiled under reflux for 2 hours. After cooling, the reaction medium is concentrated by half and extracted with 3×1.5 l of ethyl ether. The solution is evaporated to dryness and the oily residue is taken up with 160 ml of ethanol. The solution is cooled to 0° C. and 40 ml of propylene oxide is added. A white solid precipitates. The precipitate is dewatered, washed with ethanol (2×20 ml), ethyl ether (2×10 ml) and dried. White solid, 7.25 g (95.3%).

Workup

  1. temperatureunder reflux for 2 hours
  2. temperatureAfter cooling
  3. concentrationthe reaction medium is concentrated by half
  4. extractionextracted with 3×1.5 l of ethyl ether
  5. customThe solution is evaporated to dryness
  6. addition40 ml of propylene oxide is added
  7. customA white solid precipitates
  8. washwashed with ethanol (2×20 ml), ethyl ether (2×10 ml)
  9. customdried

Sources & evidence

ORD record
ord-e3db190c8d52475e935094c60257f474
Source dataset
uspto-grants-2014_04
Patent number
US08703747B2

Reaction notes

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