Hydrochloric Acid → HCID 67416696, compound

HRID 926989Notes

Reaction equation

HRID 926989 reaction equation
C([CH:3]1[CH2:6][CH2:5][C:4]1([O:10][C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[C:7]([OH:9])=[O:8])C.Cl>C(O)(=O)C>[Cl:17][C:14]1[CH:13]=[CH:12][C:11]([O:10][C:4]2([C:7]([OH:9])=[O:8])[CH2:5][CH2:6][CH2:3]2)=[CH:16][CH:15]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 66887528HCID 66887528, compound

Product 1

HCID 67416696HCID 67416696, compoundYield 87.5%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

To the product of Example 55A (320 mg, 1.26 mmol) was added glacial acetic acid (10 ml) followed by 5% aqueous hydrochloric acid (2.5 ml) and the mixture was heated to reflux for about 18 hours. The mixture was cooled and was evaporated to dryness. The residue was taken up in toluene and was evaporated to dryness two times to provide 250 mg (87%) of the title compound. MS (DCI): m/z 244 (M+NH4)+.

Workup

  1. temperaturethe mixture was heated
  2. temperatureto reflux for about 18 hours
  3. temperatureThe mixture was cooled
  4. customwas evaporated to dryness
  5. customwas evaporated to dryness two times

Sources & evidence

ORD record
ord-f1b614ad49b6467ab26f1ef37cf82468
Source dataset
uspto-grants-2016_03
Patent number
US09290444B2

Reaction notes

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