Hydrochloric Acid → HCID 21476330, compound

HRID 2293575Notes

Reaction equation

HRID 2293575 reaction equation
[CH3:1][C:2]1([CH3:30])[CH:6]2[CH2:7][CH2:8][C:3]1([CH2:13][S:14]([N:17]1[CH2:22][CH2:21][N:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[CH3:29])[CH2:19][CH2:18]1)(=[O:16])=[O:15])[C:4]([C:9]([O:11]C)=[O:10])=[CH:5]2.[OH-].[K+].Cl>CO>[CH3:1][C:2]1([CH3:30])[CH:6]2[CH2:7][CH2:8][C:3]1([CH2:13][S:14]([N:17]1[CH2:22][CH2:21][N:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[CH3:29])[CH2:19][CH2:18]1)(=[O:16])=[O:15])[C:4]([C:9]([OH:11])=[O:10])=[CH:5]2

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 21476324HCID 21476324, compound

Product 1

HCID 21476330HCID 21476330, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a stirred solution of 1-((7,7-dimethyl-2-methoxycarbonyl-bicyclo(2.2.1)hept-2-en-1-yl)methanesulfonyl)-4-(2-methylphenyl)-piperazine (1.0 g; 2.3 mmol) in MeOH (10 mL) was added a solution of 4M aqueous KOH (2.0 mL; 8.0 mmol). After 18 h, the reaction was brought to pH 1 with 5% aqueous HCl, and the solvents were removed under reduced pressure. The residue was taken up in chloroform (50 mL) and washed with water (25 mL). The organic phase was dried (MgSO4), filtered, and the solvent was removed under reduced pressure to give the hydrochloride salt of the title compound as a white foam.

Workup

  1. customthe solvents were removed under reduced pressure
  2. washwashed with water (25 mL)
  3. dry with materialThe organic phase was dried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent was removed under reduced pressure

Sources & evidence

ORD record
ord-547393995f194f48bfaa428c22ba98f4
Source dataset
uspto-grants-1997_11
Patent number
US05686454

Reaction notes

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