反应详情

To 4-(3-chlorobenzyl)-piperazine-1-carboxylic acid tert-butyl ester (20.24) (8.82 g, 28.4 mmol) is added TFA (45 mL) at ambient temperature over 5 min. After 1 h 50 min, TFA is evaporated, the residue is dissolved in 2N HCl (45 mL) and extracted with ether (2×45 mL). The aqueous layer is basified to pH 13 with 2N NaOH (60 mL) and extracted with CH2Cl2 (6×90 mL). The combined organic extracts are washed with brine (75 mL) and dried over MgSO4. The crude material obtained after filtration and concentration (5.44 g, 25.8 mmol, 91%) is used without further purification. MS (ES): m/z 211.0/213.0 (100/35) [MH+]. tR (method B)=5.1 min.

1. customAfter 1 h 50 min, TFA is evaporated
2. dissolutionthe residue is dissolved in 2N HCl (45 mL)
3. extractionextracted with ether (2×45 mL)
4. extractionextracted with CH2Cl2 (6×90 mL)
5. washThe combined organic extracts are washed with brine (75 mL)
6. dry with materialdried over MgSO4