Phosphorus oxychloride → HCID 19375601, compound

HRID 2211115Notes

Reaction equation

HRID 2211115 reaction equation
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[C:11]2[S:12][CH:13]=[CH:14][C:10]=2[C:9](=O)[NH:8][N:7]=1.P(Cl)(Cl)([Cl:18])=O>ClC(Cl)C>[Cl:18][C:9]1[N:8]=[N:7][C:6]([C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)=[C:11]2[S:12][CH:13]=[CH:14][C:10]=12

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 19375604HCID 19375604, compound

Product 1

HCID 19375601HCID 19375601, compoundYield 95.8%

Reagents, catalysts & solvents 1

HCID 63651,1-DichloroethaneSolvent

Conditions

Temperature
100 °C

Procedure

0.30 g of 7-(2-thienyl)thieno[2,3-d]pyridazine-4(5H)-one and 0.30 g of phosphorus oxychloride were dissolved in 10 ml of dichloroethane, and the solution was stirred at 100° C. for 10 hours. The reaction solution was concentrated, and a 1-N aqueous KOH solution was added thereto under cooling with ice. The solution was extracted with chloroform and dried. The solvent was distilled off, thereby obtaining 0.31 g of 4-chloro-7-(2-thienyl)thieno-[2,3-d]pyridazine.

Workup

  1. concentrationThe reaction solution was concentrated
  2. additiona 1-N aqueous KOH solution was added
  3. temperatureunder cooling with ice
  4. extractionThe solution was extracted with chloroform
  5. customdried
  6. distillationThe solvent was distilled off

Sources & evidence

ORD record
ord-2363c1ca4bd54a1ca6c7e34cf734cdeb
Source dataset
uspto-grants-1995_10
Patent number
US05462941

Reaction notes

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