反应详情

Trifluoroacetic acid (4 mL) is added to a solution of 4-[4-(6-chloro-benzo[b]thiophene-2-sulfonyl)-2-oxo-piperazin-1-ylmethyl]-piperidine-1-carboxylic acid tert-butyl ester (1.1 g, 2.0 mmol) in CH2Cl2 (15 mL). After 1 h the reaction is concentrated and the residue is dissolved in CH2Cl2 and washed with Na2CO3, dried (MgSO4) and concentrated to provide 4-(6-chloro-benzo[b]thiophene-2-sulfonyl)-1-piperidin-4-ylmethyl-piperazin-2-one. 1H NMR (300 MHz, CDCl3) δ 7.87-7.83 (m, 3H), 7.46 (dd, 1H), 3.86 (dd, 2H), 3.45 (s, 2H), 3.23 (d, 2H), 3.07 (d, 2H), 2.54 (dt, 2H), 2.39 (s, 1H), 1.83-1.75 (m, 1H), 1.56 (d, 2H), 1.24-1.11 (m, 2H); MS (Ion spray) 428 (M+H)+.

1. concentrationAfter 1 h the reaction is concentrated
2. dissolutionthe residue is dissolved in CH2Cl2
3. washwashed with Na2CO3
4. dry with materialdried (MgSO4)
5. concentrationconcentrated