Methanesulfonic Acid → HCID 19812354, compound

HRID 373315Notes

Reaction equation

HRID 373315 reaction equation
[C:1]([C:3]1[C:4]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[N:5][CH:6]=[C:7]([C:9]2[CH:14]=[CH:13][N+:12]([O-:15])=[CH:11][CH:10]=2)[CH:8]=1)#[N:2].[CH3:22][S:23]([OH:26])(=[O:25])=[O:24]>CC(C)=O>[CH3:22][S:23]([OH:26])(=[O:25])=[O:24].[C:1]([C:3]1[C:4]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[N:5][CH:6]=[C:7]([C:9]2[CH:10]=[CH:11][N+:12]([O-:15])=[CH:13][CH:14]=2)[CH:8]=1)#[N:2]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 10401503HCID 10401503, compound

Product 1

HCID 19812354HCID 19812354, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

0.3 g 3-Cyano-2-morpholino-5,4'-bipyridine-1'-oxide is dissolved in acetone with heating. The solution is allowed to cool, then treated with 0.1 ml methanesulfonic acid and concentrated under vacuum in the rotary evaporator. The oily residue is dissolved in acetone. The resulting solution is mixed with ether until crystallization, then is cooled and filtered with suction. The material filtered out is washed with acetone and ether and dried. Yield: 0.3 g (74.0% of the theoretical yield), the melting point is 151° C.-154° C.

Workup

  1. temperaturewith heating
  2. temperatureto cool
  3. concentrationconcentrated under vacuum in the rotary evaporator
  4. dissolutionThe oily residue is dissolved in acetone
  5. additionThe resulting solution is mixed with ether until crystallization
  6. temperatureis cooled
  7. filtrationfiltered with suction
  8. filtrationThe material filtered out
  9. washis washed with acetone and ether
  10. customdried
  11. customYield: 0.3 g (74.0% of the theoretical yield), the melting point is 151° C.-154° C.

Sources & evidence

ORD record
ord-e829f607340f4e09b0156ea115afbc8f
Source dataset
uspto-grants-1992_11
Patent number
US05162533

Reaction notes

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