Hydrochloric Acid → HCID 89690404, compound

HRID 2202894Notes

Reaction equation

HRID 2202894 reaction equation
[Cl:1][C:2]1[CH:22]=[CH:21][C:5]([CH2:6][O:7][C:8]2[CH:13]=[N:12][N:11](C3CCCCO3)[C:10](=[O:20])[CH:9]=2)=[CH:4][CH:3]=1.Cl>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][O:7][C:8]2[CH:13]=[N:12][NH:11][C:10](=[O:20])[CH:9]=2)=[CH:21][CH:22]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 89690348HCID 89690348, compound

Product 1

HCID 89690404HCID 89690404, compoundYield 90.4%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a stirred suspension of 5-((4-chlorobenzyl)oxy)-2-(tetrahydro-2H-pyran-2-yl)pyridazin-3(2H)-one (210 mg) in MeOH (5 ml) was added conc. HCl (0.5 ml) at room temperature, and then the reaction mixture was heated at reflux for 3 h. The mixture was cooled to room temperature, concentrated in vacuo and neutralized with saturated NaHCO3 (20 ml). The resulting precipitate was collected by filtration, washed with water and dried in vacuo to give the title compound (140 mg) as an off-white solid.

Workup

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for 3 h
  3. concentrationconcentrated in vacuo
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with water
  6. customdried in vacuo

Sources & evidence

ORD record
ord-97cf61ff95d54030ac7af30bbe2d1773
Source dataset
uspto-grants-2016_06
Patent number
US09365540B2

Reaction notes

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