Phosphorus oxychloride → HCID 13424594, compound

HRID 372704Notes

Reaction equation

HRID 372704 reaction equation
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:10]([CH3:16])=[CH:11][C:12](=O)[NH:13][N:14]=2)=[CH:5][CH:4]=1)#[N:2].P(Cl)(Cl)([Cl:19])=O>>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:14]=[N:13][C:12]([Cl:19])=[CH:11][C:10]=2[CH3:16])=[CH:5][CH:4]=1)#[N:2]

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 13424593HCID 13424593, compound

Product 1

HCID 13424594HCID 13424594, compound

Procedure

A 2.0 portion of 6-(p-cyanophenyl)-5-methyl-3(2H)-pyridazinone and 10 ml. of phosphorus oxychloride are heated at steam bath temperature for 4 hours. The reaction mixture is poured into crushed ice and the resulting solid, after decomposition of the unreacted phosphorus oxychloride, is recovered by filtration, washed with water and dried. This product is recrystallized several times from methanol giving 6-(p-cyanophenyl)-5-methyl-3-chloropyridazine, m.p. 218°-220° C.

Workup

  1. additionThe reaction mixture is poured
  2. custominto crushed ice
  3. filtrationthe resulting solid, after decomposition of the unreacted phosphorus oxychloride, is recovered by filtration
  4. washwashed with water
  5. customdried
  6. customThis product is recrystallized several times from methanol

Sources & evidence

ORD record
ord-475ac7d1a1ac49ee975947e4c4dcf4eb
Source dataset
uspto-grants-1978_05
Patent number
US04092311

Reaction notes

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