Reaktion #71652

Reaktionsgleichung

1,1-dimethylethyl (3S)-4-[(4-cyano-2-methylphenyl)sulfonyl]-3-methyl-1-piperazinecarboxylate

TFA

→

title compound

Ausbeute 91.5%

3-methyl-4-{[(2S)-2-methyl-1-piperazinyl]sulfonyl}benzonitrile

Ausbeute 91.5%

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated under vacuum
2. 2
   Sonstigeazeotroping with toluene (25 ml)
3. 3
   workup.DISSOLUTIONThe residue was dissolved in MeOH (20 ml)
4. 4
   workup.ADDITIONadded to an SCX-2 cartridge (50 g)
5. 5
   Waschenwashing with MeOH
6. 6
   WaschenThe product was eluted with 2M NH3 in MeOH
7. 7
   Einengenconcentration under vacuum

Vorschrift

A solution of 1,1-dimethylethyl (3S)-4-[(4-cyano-2-methylphenyl)sulfonyl]-3-methyl-1-piperazinecarboxylate (may be prepared as described in Description 16) (3.71 g, 9.78 mmol) and TFA (5.00 ml, 64.9 mmol) in dry DCM (15 ml) was stirred at rt for 1 h, then concentrated under vacuum, azeotroping with toluene (25 ml). The residue was dissolved in MeOH (20 ml) and added to an SCX-2 cartridge (50 g), washing with MeOH. The product was eluted with 2M NH3 in MeOH; concentration under vacuum gave the title compound as a white solid (2.50 g).

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