Hydrochloric Acid → HCID 178517150, compound

HRID 359923Notes

Reaction equation

HRID 359923 reaction equation
CS[C:3]1[N:4]=[C:5]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=[C:6]2[N:7]=1.Cl.C([OH:16])C.C(=O)([O-])O.[Na+]>O>[OH:16][C:3]1[N:4]=[C:5]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=[C:6]2[N:7]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 516892Sodium BicarbonateHCID 151230382-Methylthiocycloheptimidazole

Product 1

HCID 178517150HCID 178517150, compoundYield 80.3%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

In accordance with the method described in Journal of the Americal Chemical Society, Vol. 76, pages 3352 to 3353 (1954), 60 g of 2-methylthiocycloheptimidazole, as obtained in Example 1-(c), was added to 300 ml of concentrated hydrochloric acid (hydrogen chloride content: 35%) and heated under reflux for 2 hours and 30 minutes. Next, 500 ml of ethanol was added and everything was stirred at room temperature, and then the crystals precipitated were separated by filtration. The crystals thus obtained were dissolved in 0.5 liter of water, and sodium hydrogencarbonate was added to adjust the pH thereof to about pH 7 or so. The crystals precipitated were separated by filtration, washed with water and then dried. 40 g of pale yellow crystals were obtained.

Workup

  1. temperatureheated
  2. temperatureunder reflux for 2 hours and 30 minutes
  3. customthe crystals precipitated
  4. customwere separated by filtration
  5. customThe crystals thus obtained
  6. customThe crystals precipitated
  7. customwere separated by filtration
  8. washwashed with water
  9. customdried

Sources & evidence

ORD record
ord-9260286f561644188a9b2366f933cd7c
Source dataset
uspto-grants-1991_03
Patent number
US05003077

Reaction notes

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