Fuming sulfuric acid → HCID 178527632, compound

HRID 2210422Notes

Reaction equation

HRID 2210422 reaction equation
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][N:3]=1.[OH:9][S:10](O)(=[O:12])=[O:11].O=S(=O)=O>CO.CC(C)=O>[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[C:5]([S:10]([OH:12])(=[O:11])=[O:9])=[CH:4][N:3]=1

Participants

4

Reactant 2

HCID 24681Fuming sulfuric acidHCID 178516518HCID 178516518, compound

Product 1

HCID 178527632HCID 178527632, compound

Reagents, catalysts & solvents 1

HCID 21894497Aceton-methanolSolvent

Conditions

Temperature
-50 °C

Procedure

5 g of 2,4-dihydroxypyridine are slowly added, at a temperature in the region of -10° C., to 12.5 cm3 of sulfuric oleum containing 20% SO3 and containing 250 mg of HgSO4. After having left to return to ordinary temperature, the mixture is progressively brought to 150° C. and then maintained at this temperature for 16 hours. The mixture is poured onto a MeOH/acetone (50/50) mixture cooled to around -50° C. A beige precipitate is formed which is recrystallized from the same MeOH/acetone mixture.

Workup

  1. waitAfter having left
  2. customis progressively brought to 150° C.
  3. temperaturemaintained at this temperature for 16 hours
  4. customA beige precipitate is formed which
  5. customis recrystallized from the same MeOH/acetone mixture

Sources & evidence

ORD record
ord-333d96c923bc4b2cb667e10086882a7e
Source dataset
uspto-grants-1995_10
Patent number
US05459138

Reaction notes

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