Hydrochloric Acid → HCID 85826896, compound

HRID 1254957Notes

Reaction equation

HRID 1254957 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-ea6a390f11f543fbae7d591a621f148f
Source dataset
uspto-grants-2013_06
Patent number
US08455659B2

Reaction notes

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