Ether hydrochloride → 1-[(2R,6S)-2,6-Dimethylpiperazin-1-yl]ethan-1-one hydrochloride

HRID 885849Notes

Reaction equation

HRID 885849 reaction equation
C(OC([N:8]1[CH2:13][C@@H:12]([CH3:14])[N:11]([C:15](=[O:17])[CH3:16])[C@@H:10]([CH3:18])[CH2:9]1)=O)(C)(C)C.[ClH:19].CCOCC>C(Cl)Cl>[ClH:19].[CH3:14][C@@H:12]1[CH2:13][NH:8][CH2:9][C@H:10]([CH3:18])[N:11]1[C:15](=[O:17])[CH3:16]

Participants

4

Reactant 2

HCID 10953452Ether hydrochlorideHCID 57526729HCID 57526729, compound

Product 1

HCID 670491651-[(2R,6S)-2,6-Dimethylpiperazin-1-yl]ethan-1-one hydrochloride

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

(3S,5R)-4-Acetyl-3,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester (450 mg, 1.75 mmol) was dissolved in DCM (10 ml) and acidified with HCl/Et2O. The mixture was stirred at room temperature for two days. The resulting solid was filtered to give 190 mg of 1-((2R,6S)-2,6-dimethyl-piperazin-1-yl)ethanone hydrochloride. The mother liquors were treated with HCl/Et2O for 4 h and the resulting solid was filtered to give additional 43 mg of the title compound as hydrochloric salt.

Workup

  1. filtrationThe resulting solid was filtered

Sources & evidence

ORD record
ord-65965ee40c67498fba2337f22c12f5c3
Source dataset
uspto-grants-2012_08
Patent number
US08242175B2

Reaction notes

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