Hydrochloric Acid → HCID 67153007, compound

HRID 2368204Notes

Reaction equation

HRID 2368204 reaction equation
C([NH:14][P:15]([CH2:18][C:19]1[CH:23]=[CH:22][S: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:23]=[CH:22][S:21][CH:20]=1)(=[O:16])[OH:17]

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 86653628HCID 86653628, compound

Product 1

HCID 67153007HCID 67153007, compound

Conditions

Temperature
0 °C

Procedure

A mixture of 15 g of the compound from step 1 and 122 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 120 ml of ethanol. The solution is cooled to 0° C. and 30 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, 7.32 g (95.1%).

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. addition30 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-4b6c85345b294dada2d0d486b85118df
Source dataset
uspto-grants-2014_04
Patent number
US08703747B2

Reaction notes

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