Methanesulfonic Acid → HCID 136331495, compound

HRID 274437Notes

Reaction equation

HRID 274437 reaction equation
[N:1]1[CH:6]=[CH:5][C:4]([C:7]([C:9]2[CH:14]=[C:13]([N+:15]([O-:17])=[O:16])[C:12]([OH:18])=[C:11]([OH:19])[CH:10]=2)=[O:8])=[CH:3][CH:2]=1.[CH3:20][S:21]([OH:24])(=[O:23])=[O:22]>CO>[CH3:20][S:21]([OH:24])(=[O:23])=[O:22].[N:1]1[CH:6]=[CH:5][C:4]([C:7]([C:9]2[CH:14]=[C:13]([N+:15]([O-:17])=[O:16])[C:12]([OH:18])=[C:11]([OH:19])[CH:10]=2)=[O:8])=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 135665314125629-00-7

Product 1

HCID 136331495HCID 136331495, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

13.2 g of 3,4-dihydroxy-5-nitrophenyl 4-pyridyl ketone are suspended in 500 ml of methanol and treated while stirring with 4.88 g of methanesulfonic acid. The suspension is heated under reflux for 60 minutes. It is subsequently cooled to 10°, the crystals are filtered under suction and washed twice with 30 ml of methanol each time. There is obtained 3,4-dihydroxy-5-nitrophenyl 4-pyridyl ketone methanesulfonate of m.p. 260°-261° (dec.).

Workup

  1. additiontreated
  2. temperatureThe suspension is heated
  3. temperatureunder reflux for 60 minutes
  4. temperatureIt is subsequently cooled to 10°
  5. filtrationthe crystals are filtered under suction
  6. washwashed twice with 30 ml of methanol each time

Sources & evidence

ORD record
ord-4e34fa4bddcd4bfca538a22d8a28b843
Source dataset
uspto-grants-1995_02
Patent number
US05389653

Reaction notes

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