Phosphorus oxychloride → 3,4,5-Trichloropyridazine
Reaction equation
[Cl:1][C:2]1[C:3](=O)[NH:4][N:5]=[CH:6][C:7]=1[Cl:8].O=P(Cl)(Cl)[Cl:12]>>[Cl:12][C:3]1[N:4]=[N:5][CH:6]=[C:7]([Cl:8])[C:2]=1[Cl:1]Participants
3
Procedure
A stirred solution of 4,5-dichloro-2,3-dihydro-3-pyridazinone (15.00 g, 90.92 mmol) in POCl3 (100 mL) was refluxed for 1.5 h, then concentrated in vacuo. The residue was dissolved in CH2Cl2 (400 mL), washed with water (100 mL), dried over Na2SO4, filtered and concentrated to give 3,4,5-trichloropyridazine. M.S.(M+1):185.00
Workup
- concentrationconcentrated in vacuo
- dissolutionThe residue was dissolved in CH2Cl2 (400 mL)
- washwashed with water (100 mL)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-44e5693979c348a580ef81af0ea52895
- Source dataset
- uspto-grants-2006_05
- Patent number
- US07053089B2
Reaction notes
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