Potassium Hydroxide → HCID 21331692, compound

HRID 1390923Notes

Reaction equation

HRID 1390923 reaction equation
[CH3:1][S:2](Cl)(=[O:4])=[O:3].O[N:7]1[C:12]([OH:13])=[CH:11][CH:10]=[CH:9][NH:8]1.[OH-:14].[K+]>O>[CH3:1][S:2]([O:4][C:9]1[CH:10]=[CH:11][C:12](=[O:13])[NH:7][N:8]=1)(=[O:14])=[O:3]

Participants

5

Reactant 3

HCID 14797Potassium HydroxideHCID 31297Methanesulfonyl chlorideHCID 18615901HCID 18615901, compound

Product 1

HCID 21331692HCID 21331692, compoundYield 51%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
-10 °C

Procedure

102.9 g (0.9 mole) of methanesulfonic acid chloride were added dropwise at 0° C. to a solution of 100.8 g (0.9 mole) of 1,6-dihydroxypyridazine and 50.4 g (0.9 mole) of potassium hydroxide in 500 ml of water. The mixture was allowed to react for a further hour at 20° C. and was then cooled to -10° C., and the precipitate formed was filtered off. After recrystallization from acetonitrile, 87 g (51% of theory) of 1,6-dihydro-3-methylsulfonyloxy-6-oxopyridazine were obtained in the form of colorless crystals of melting point 148° C. ##STR194##

Workup

  1. customto react for a further hour at 20° C.
  2. customthe precipitate formed
  3. filtrationwas filtered off
  4. customAfter recrystallization from acetonitrile

Sources & evidence

ORD record
ord-a702533e51e14e12a1a02d0ea4998e4c
Source dataset
uspto-grants-1979_02
Patent number
US04140768

Reaction notes

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