Phosphorus oxychloride → HCID 15225040, compound

HRID 2211098Notes

Reaction equation

HRID 2211098 reaction equation
[CH:1]1([C:7]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10](=O)[NH:9][N:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.P(Cl)(Cl)([Cl:20])=O>ClC(Cl)C>[Cl:20][C:10]1[C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:7]([CH:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)=[N:8][N:9]=1

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 10263181HCID 10263181, compound

Product 1

HCID 15225040HCID 15225040, compound

Reagents, catalysts & solvents 1

HCID 63651,1-DichloroethaneSolvent

Conditions

Temperature
100 °C

Procedure

1.0 g of 4-cyclohexyl-1-phthalazinone and 5 ml of phosphorus oxychloride were dissolved in 10 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 1.1 g of 1-chloro-4-cyclo-hexylphthalazine.

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-16053e4966dd4e9da7cbf183f87346a3
Source dataset
uspto-grants-1995_10
Patent number
US05462941

Reaction notes

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