Hydrochloric Acid → HCID 85826896, compound

HRID 623792Notes

Reaction equation

HRID 623792 reaction equation
[C:1](OC)(=[O:3])C.[C:6](#[N:14])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].[ClH:15].CC1CCCCC1>CO>[ClH:15].[C:6](=[NH:14])([O:3][CH3:1])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 6584Methyl AcetateHCID 7962MethylcyclohexaneHCID 31286Octanenitrile

Product 1

HCID 85826896HCID 85826896, compoundYield 93.4%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
0 °C

Procedure

Methanol (2.81 g) and methyl acetate (30 ml) were added to octanenitrile (10.00 g), and the mixture was cooled to 0° C. Hydrogen chloride (7.50 g) was added and the mixture was stirred for 25 hours at the same temperature. Methylcyclohexane (60 ml) was added to the reaction solution, and then the solvent was distilled off under reduced pressure. Methylcyclohexane (20 ml) was added to the residue, the mixture was stirred for 1.5 hours at room temperature, and then crystals were filtered. The crystals were washed with methylcyclohexane and dried under reduced pressure to give the title compound as a white solid (14.45 g, 93.4% yield).

Workup

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionMethylcyclohexane (20 ml) was added to the residue
  3. stirringthe mixture was stirred for 1.5 hours at room temperature
  4. filtrationcrystals were filtered
  5. washThe crystals were washed with methylcyclohexane
  6. customdried under reduced pressure

Sources & evidence

ORD record
ord-2699318abce84518a66aa7aa220e6422
Source dataset
uspto-grants-2016_04
Patent number
US09303008B2

Reaction notes

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