Sulfuric Acid → HCID 20489818, compound

HRID 2072018Notes

Reaction equation

HRID 2072018 reaction equation
[C:1]([C:3]1([N:9]([CH3:11])[CH3:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)#[N:2].S(=O)(=O)(O)[OH:13]>O.O.O.O.O.O.O.O.[OH-].[Ba+2].[OH-]>[CH3:10][N:9]([CH3:11])[C:3]1([C:1]([NH2:2])=[O:13])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1

Participants

4

Reactant 2

HCID 1118Sulfuric AcidHCID 1011881-(Dimethylamino)cyclohexanecarbonitrile

Product 1

HCID 20489818HCID 20489818, compound

Reagents, catalysts & solvents 1

HCID 17749109Barium hydroxide, octahydrateSolvent

Procedure

1-Cyano-N,N-dimethyl cyclohexylamine (10 g.) was added portionwise to conc. sulphuric acid (20 ml.) and the solution left for 15 minutes. The cooled solution was diluted with ice-cold water and neutralised with barium hydroxide octahydrate. The mixture was filtered on hyflo and the filtrate evaporated to dryness when the residual oil (9.1 g., 81%) crystallised on standing. Recrystallisation from petrol (80/100) afforded 1-dimethylamino cyclohexane carboxamide m.p. 65°69°.

Workup

  1. filtrationThe mixture was filtered on hyflo
  2. customthe filtrate evaporated to dryness when the residual oil (9.1 g., 81%)
  3. customcrystallised
  4. customRecrystallisation from petrol (80/100)

Sources & evidence

ORD record
ord-fbae10c4b1074ad4b208a013766c7856
Source dataset
uspto-grants-1977_09
Patent number
US04049663

Reaction notes

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