Methanesulfonic Acid → HCID 178505257, compound

HRID 1700657Notes

Reaction equation

HRID 1700657 reaction equation
[Cl:1][C:2]1[S:3][C:4]([Cl:23])=[CH:5][C:6]=1[CH:7]1[CH2:16][C:15]2[N:14]=[CH:13][CH:12]=[C:11]([CH3:17])[C:10]=2[C:9](=[N:18][NH:19][C:20]([NH2:22])=[NH:21])[CH2:8]1.[CH3:24][S:25]([OH:28])(=[O:27])=[O:26]>C(O)C>[OH2:26].[CH3:24][S:25]([OH:28])(=[O:27])=[O:26].[Cl:1][C:2]1[S:3][C:4]([Cl:23])=[CH:5][C:6]=1[CH:7]1[CH2:16][C:15]2[N:14]=[CH:13][CH:12]=[C:11]([CH3:17])[C:10]=2[C:9](=[N:18][NH:19][C:20]([NH2:22])=[NH:21])[CH2:8]1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 178428123HCID 178428123, compound

Product 1

HCID 178505257HCID 178505257, compoundYield 107.7%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of (−)-7-(2,5-dichlorothiophen-3-yl)-5-guanidinoimino-4-methyl-5,6,7,8-tetrahydroquinoline (0.8 g) in ethanol (20 ml) was added methanesulfonic acid (0.37 g), and the mixture was concentrated under reduced pressure. To the residue was added water (1 ml), and the mixture was concentrated to precipitate crystals, which were filtered and washed with ethanol. The thus obtained crystals were dried to give (−)-7-(2,5-dichlorothiophen-3-yl)-5-guanidinoimino-4-methyl-5,6,7,8-tetrahydroquinoline methanesulfonate monohydrate (Compound 114) (1.0 g).

Workup

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionTo the residue was added water (1 ml)
  3. concentrationthe mixture was concentrated
  4. customto precipitate crystals, which
  5. filtrationwere filtered
  6. washwashed with ethanol
  7. customThe thus obtained crystals were dried

Sources & evidence

ORD record
ord-97ce3df5508f48859ef7109e6ca31a0b
Source dataset
uspto-grants-2002_02
Patent number
US06350749B1

Reaction notes

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