Phosphorus oxychloride → HCID 19375606, compound

HRID 2211101Notes

Reaction equation

HRID 2211101 reaction equation
[S:1]1[CH:5]=[CH:4][C:3]([C:6]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9](=O)[NH:8][N:7]=2)=[CH:2]1.P(Cl)(Cl)([Cl:19])=O>ClC(Cl)C>[Cl:19][C:9]1[C:10]2[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:6]([C:3]2[CH:4]=[CH:5][S:1][CH:2]=2)=[N:7][N:8]=1

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 19375607HCID 19375607, compound

Product 1

HCID 19375606HCID 19375606, compound

Reagents, catalysts & solvents 1

HCID 63651,1-DichloroethaneSolvent

Conditions

Temperature
100 °C

Procedure

500 mg of 4-(3-thienyl)-1-phthalazinone and 3 ml of phosphorus oxychloride were dissolved in 6 ml of dichloroethane, and the solution was stirred at 100° C. for 4 hours. The reaction solution was distilled off, and a 1-N aqueous NaOH solution was added thereto under cooling with ice. The solution was extracted with chloroform and dried over magnesium sulfide. The solvent was then distilled off, thereby obtaining 515 mg of 1-chloro-4-(3-thienyl)phthalazine.

Workup

  1. distillationThe reaction solution was distilled off
  2. additiona 1-N aqueous NaOH solution was added
  3. temperatureunder cooling with ice
  4. extractionThe solution was extracted with chloroform
  5. dry with materialdried over magnesium sulfide
  6. distillationThe solvent was then distilled off

Sources & evidence

ORD record
ord-70d91eeaabdc4a6bb4faa7d1f9c5bdd3
Source dataset
uspto-grants-1995_10
Patent number
US05462941

Reaction notes

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