反应详情

A solution of 1,1-dimethylethyl (2S)-4-[(4-cyano-2-methylphenyl)sulfonyl]-2-methyl-1-piperazinecarboxylate (may be prepared as described in Description 10) (2.88 g, 7.59 mmol) and TFA (10 ml, 130 mmol) in dry DCM (10 ml) was stirred at room temperature for 1 hour, then concentrated in vacuo, azeotroping with toluene (25 ml) to give a brown oil. This was partitioned between DCM (50 ml) and saturated aqueous NaHCO3 (50 ml), then the aqueous layer was extracted with DCM (50 ml). The combined organic layers were passed through a hydrophobic frit and concentrated in vacuo to give the title compound as a yellow oil (2.29 g).

1. concentrationconcentrated in vacuo
2. customazeotroping with toluene (25 ml)
3. customto give a brown oil
4. customThis was partitioned between DCM (50 ml) and saturated aqueous NaHCO3 (50 ml)
5. extractionthe aqueous layer was extracted with DCM (50 ml)
6. concentrationconcentrated in vacuo