反应详情

A mixture of 2,2-dimethylpiperazine-1-carboxylic acid tert-butyl ester (1.0 g, 4.60 mmol) and NEt3 (1.3 mL, 9.34 mmol) in DCM (11 mL) was cooled to 0° C. before the drop wise addition of a solution of methanesulfonyl chloride (580 mg, 5.00 mmol) in DCM (2 mL). The resulting mixture was warmed to r.t. and allowed to stir for 30 min before H2O was added. The organic phase was dried (phase separator) and concentrated in vacuo. The resulting residue was dissolved in DCM (10 mL) and TFA (2 mL) was added. The resulting mixture was allowed to stir at r.t. for 30 min then concentrated in vacuo. The resulting residue was partitioned between DCM and sat. aq. NaHCO3 and the aqueous phase was loaded onto an Isolute® SCX-2 cartridge which was washed with H2O and MeOH. The product was eluted with 2M NH3/MeOH affording the title compound (800 mg, 90%). LCMS (method A): RT 0.29 min [M+H]+ 193.3

1. additionwas added
2. customThe organic phase was dried (phase separator)
3. concentrationconcentrated in vacuo
4. dissolutionThe resulting residue was dissolved in DCM (10 mL)
5. additionTFA (2 mL) was added
6. concentrationthen concentrated in vacuo
7. customThe resulting residue was partitioned between DCM and sat. aq. NaHCO3
8. washwas washed with H2O and MeOH
9. washThe product was eluted with 2M NH3/MeOH affording the title compound (800 mg, 90%)
10. customRT 0.29 min [M+H]+ 193.3