HCID 178422887, compound → HCID 178422888, compound

HRID 223592Notes

Reaction equation

HRID 223592 reaction equation
C([C:4]1[N:9]=[N:8][C:7]2[C:10]3[CH:16]=[CH:15][C:14]([CH3:17])=[N:13][C:11]=3[S:12][C:6]=2[C:5]=1[OH:18])(O)=O>C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1.CCCCCC>[OH:18][C:5]1[C:6]2[S:12][C:11]3[N:13]=[C:14]([CH3:17])[CH:15]=[CH:16][C:10]=3[C:7]=2[N:8]=[N:9][CH:4]=1

Participants

4

Reactant 1

HCID 178422887HCID 178422887, compound

Product 1

HCID 178422888HCID 178422888, compoundYield 66.5%

Reagents, catalysts & solvents 2

HCID 8058HexaneSolventHCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)Solvent

Conditions

Temperature
225 °C

Procedure

A mixture of 2.4 g (0.009 mol) of 3-carboxy-4-hydroxy-7-methylpyrido[3',2':4,5]-thieno[3,2-C]pyridazine in 70 ml of Dowtherm-A was stirred at 225° C. for 30 minutes. It was cooled, diluted with hexane and filtered. The crude product was crystallized by 5% NaOH/HOAC giving 1.3 g (65%) of 4-hydroxy-7-methylpyrido[3',2':4,5]thieno[3,2-C]pyridazine, m.p.>300° C.

Workup

  1. temperatureIt was cooled
  2. filtrationfiltered
  3. customThe crude product was crystallized by 5% NaOH/HOAC

Sources & evidence

ORD record
ord-db23a7df47ce43e88181e32cd36573c0
Source dataset
uspto-grants-1982_10
Patent number
US04355164

Reaction notes

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