Hydrochloric Acid → HCID 85826896, compound

HRID 626093Notes

Reaction equation

HRID 626093 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

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-4bb3c398014a4fce906e929502cc716f
Source dataset
uspto-grants-2016_04
Patent number
US09309214B2

Reaction notes

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