Hydrochloric Acid → HCID 69219769, compound

HRID 32234Notes

Reaction equation

HRID 32234 reaction equation
[Cl:1][CH2:2][C@@H:3]1[CH2:5][C@H:4]1[CH2:6][N:7]1[CH2:12][CH2:11][N:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[CH:19]2[CH2:24][C:23]([CH3:26])([CH3:25])[CH2:22][C:21]([CH3:28])([CH3:27])[CH2:20]2)[CH2:9][CH2:8]1.Cl>ClCCl.C(OCC)(=O)C>[ClH:1].[Cl:1][CH2:2][C@@H:3]1[CH2:5][C@H:4]1[CH2:6][N:7]1[CH2:8][CH2:9][N:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[CH:19]2[CH2:24][C:23]([CH3:26])([CH3:25])[CH2:22][C:21]([CH3:28])([CH3:27])[CH2:20]2)[CH2:11][CH2:12]1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 59769393trans-1-(2-Chloromethylcyclopropylmethyl)-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine

Product 1

HCID 69219769HCID 69219769, compoundYield 212.4%

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolventHCID 8857Ethyl AcetateSolvent

Procedure

To trans-1-(2-chloromethylcyclopropylmethyl)-4-[2-(3,3,5,5-tetramethylcyclohexyl)-phenyl]piperazine (19 mg) produced in Example (94a) dissolved in dichloromethane was added a 4N solution of hydrogen chloride in ethyl acetate. Nitrogen was then blown to the solution to remove the solvent. Diethyl ether was added to the obtained residue to produce a solid, which was then triturated by sonication. The supernatant diethyl ether solution was removed and the obtained solid residue was dried by blowing nitrogen, to give 22 mg of the title compound as a light red solid.

Workup

  1. customto remove the solvent
  2. additionDiethyl ether was added to the obtained residue
  3. customto produce a solid, which
  4. customwas then triturated by sonication
  5. customThe supernatant diethyl ether solution was removed
  6. customthe obtained solid residue was dried

Sources & evidence

ORD record
ord-8cca56d67a9a4c18b9a02615f815773d
Source dataset
uspto-grants-2008_09
Patent number
US07425554B2

Reaction notes

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