反应详情

温度

50 °C

To the solution of 1,1-dimethylethyl 4-(2-fluoroethyl)-1-piperazinecarboxylate (from a different batch than previously described) (160 g, 0.68 mol) in MeOH (500 mL) was added HCl/MeOH (5M, 1000 mL), and the mixture was heated at 50° C. for 1 h before evaporating most of the solvent. The residue was filtered and washed with MeOH to give the title compound of Step B (122 g, 87% yield). 1H NMR (400 MHz, D2O) δ ppm 3.60-3.78 (m, 10H), 4.80 (t, J=4.4 Hz, 1H), 4.92 (t, J=4.4 Hz, 1H)

1. custombefore evaporating most of the solvent
2. filtrationThe residue was filtered
3. washwashed with MeOH