反应详情

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).

1. concentrationconcentrated under vacuum
2. customazeotroping with toluene (25 ml)
3. dissolutionThe residue was dissolved in MeOH (20 ml)
4. additionadded to an SCX-2 cartridge (50 g)
5. washwashing with MeOH
6. washThe product was eluted with 2M NH3 in MeOH
7. concentrationconcentration under vacuum