Potassium Carbonate → HCID 10630595, compound

HRID 279793Notes

Reaction equation

HRID 279793 reaction equation
[CH3:1][CH:2]1[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][C:3]1=[O:9].[N-:10]=[N+]=[N-].[Na+].C(=O)([O-])[O-].[K+].[K+]>Cl>[CH3:1][CH:2]1[NH:10][C:3](=[O:9])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 33557Sodium AzideHCID 5435032-Methylcycloheptanone

Product 1

HCID 10630595HCID 10630595, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

Cool a solution of 17 g 2-methylcycloheptanone in 75 ml concentrated hydrochloric acid and add protionwise 13.2 g sodium azide. Stir the reaction of 0° for 1 hour then at room temperature for 2 hours. Add the reaction to 150 ml ice water, bring to pH 7 with potassium carbonate and extract with chloroform. Treat the extracts with charcoal, dry over MgSO4, filter and concentrate to obtain crude 8-methylperhydroazocin-2-one. Obtain a pure product by recrystallization from hexane (m.p. 70-73).

Workup

  1. customthe reaction of 0° for 1 hour
  2. additionAdd
  3. extractionextract with chloroform
  4. additionTreat the extracts with charcoal
  5. dry with materialdry over MgSO4
  6. filtrationfilter
  7. concentrationconcentrate

Sources & evidence

ORD record
ord-3323d3aafa714d1fb3c8cebb4d35bb21
Source dataset
uspto-grants-1986_05
Patent number
US04587050

Reaction notes

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