Phosphorus oxychloride → HCID 23153698, compound

HRID 1990786Notes

Reaction equation

HRID 1990786 reaction equation
P(Cl)(Cl)([Cl:3])=O.[CH3:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:15]3[CH:24]=[CH:23][N:22]=[CH:21][C:16]=3[C:17](=O)[NH:18][N:19]=2)=[CH:10][CH:9]=1>O>[Cl:3][C:17]1[N:18]=[N:19][C:14]([C:11]2[CH:12]=[CH:13][C:8]([O:7][CH3:6])=[CH:9][CH:10]=2)=[C:15]2[CH:24]=[CH:23][N:22]=[CH:21][C:16]=12

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 23153685HCID 23153685, compound

Product 1

HCID 23153698HCID 23153698, compoundYield 92%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

With cooling with ice, 2.5 ml of phosphorus oxychloride was added to 2.53 g (10.0 mmol) of 1-(4-methoxyphenyl)-3H-pyrido[3,4-d]pyridazin-4-on, and the reaction liquid was stirred under reflux for 6 hours. Water was added to the reaction liquid, extracted with chloroform, and the organic layer was washed with saturated saline water. This was dried with anhydrous sodium chloride, and concentrated under reduced pressure to obtain 2.50 g (yield: 92%) of 4-chloro-1-(4-methoxyphenyl)-pyrido[3,4-d]pyridazine as a brown solid.

Workup

  1. customthe reaction liquid
  2. temperatureunder reflux for 6 hours
  3. extractionextracted with chloroform
  4. washthe organic layer was washed with saturated saline water
  5. dry with materialThis was dried with anhydrous sodium chloride
  6. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-8b2301bcbe98440797ab187838e98aec
Source dataset
uspto-grants-2010_01
Patent number
US07645756B2

Reaction notes

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