Phosphorus oxychloride → HCID 19375609, compound

HRID 2211106Notes

Reaction equation

HRID 2211106 reaction equation
[CH3:1][C:2]1[CH:3]=[C:4]([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)[S:5][CH:6]=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]([C:4]2[S:5][CH:6]=[C:2]([CH3:1])[CH:3]=2)=[N:8][N:9]=1

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 510510764-(4- methylthiophen-2-yl)phthalazin-1(2H)-one

Product 1

HCID 19375609HCID 19375609, compound

Reagents, catalysts & solvents 1

HCID 63651,1-DichloroethaneSolvent

Conditions

Temperature
100 °C

Procedure

200 mg of 4-(4-methyl-2-thienyl)phthalazinone and 2 ml of phosphorus oxychloride were dissolved in 4 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, dried and concentrated to obtain 206 mg of 1-chloro-4-(4-methyl-2-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. customdried
  6. concentrationconcentrated

Sources & evidence

ORD record
ord-63d43e22d86b47dfbb9f3e0747cdcc16
Source dataset
uspto-grants-1995_10
Patent number
US05462941

Reaction notes

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