Hydrochloric Acid → HCID 11718083, compound

HRID 604836Notes

Reaction equation

HRID 604836 reaction equation
[CH:1]1([CH2:4][N:5]2[CH2:10][CH2:9][N:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[CH:17]3[CH2:22][C:21]([CH3:24])([CH3:23])[CH2:20][C:19]([CH3:26])([CH3:25])[CH2:18]3)[CH2:7][CH2:6]2)[CH2:3][CH2:2]1.[ClH:27].C(OCC)(=O)C>ClCCl>[ClH:27].[CH:1]1([CH2:4][N:5]2[CH2:6][CH2:7][N:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[CH:17]3[CH2:18][C:19]([CH3:26])([CH3:25])[CH2:20][C:21]([CH3:24])([CH3:23])[CH2:22]3)[CH2:9][CH2:10]2)[CH2:3][CH2:2]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 11302685859217-52-0

Product 1

HCID 11718083HCID 11718083, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

1-Cyclopropylmethyl-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (147 mg, 0.415 mmol) obtained in Example 2 was dissolve in dichloromethane (3 mL), and a 4N solution of hydrogen chloride in ethyl acetate (0.11 mL, 0.456 mmol) was added to the mixture under a nitrogen atmosphere. This was stirred at room temperature for 15 minutes, the solvent was removed under reduced pressure. To the obtained reside was added ethyl acetate (13 mL), followed by stirring at an external temperature of 100° C. for 1 hour to form a thoroughly dissolved state. Then this solution was allowed to cool down to room temperature, followed by stirring for 19 hours 45 minutes. Precipitated hydrochloride was collected by filtration to give 134 mg of the title compound as colorless crystals.

Workup

  1. customthe solvent was removed under reduced pressure
  2. additionTo the obtained reside was added ethyl acetate (13 mL)
  3. stirringby stirring at an external temperature of 100° C. for 1 hour
  4. customto form a thoroughly dissolved state
  5. temperatureto cool down to room temperature
  6. stirringby stirring for 19 hours 45 minutes
  7. filtrationPrecipitated hydrochloride was collected by filtration

Sources & evidence

ORD record
ord-d9688751c5bb4a94a643a05d44816e6a
Source dataset
uspto-grants-2011_03
Patent number
US07910734B2

Reaction notes

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