反应详情

Dimethylamino-acetyl chloride (0.14 g, 0.86 mmol) and (4-piperidin-4-yl-phenyl)-carbamic acid tert-butyl ester (0.20 g, 0.72 mmol) were combined in CH2Cl2 (5 mL) and triethylamine (0.21 g, 2.2 mmol) was added. After 6 h, water (5 mL) was added. The reaction mixture was extracted with CH2Cl2 (3×5 mL) and the combined organic extracts were dried (MgSO4) and concentrated. The compound was found to be unstable on silica and therefore carried on without further purification. 1H NMR (400 MHz, CDCl3) δ (ppm): 9.04 (s, 1H), 7.52 (d, 2H, J=8.5 Hz), 7.16 (d, 2H, J=8.5 Hz), 3.06 (s 2H), 2.76-2.82(m, 2H), 2.59-2.65 (m, 1H), 2.37 (s, 6H), 1.78-1.81 (m, 2H), 1.54-1.64 (m, 2H), 1.48 (s, 9H), 1.30 (br s, 2H).

1. extractionThe reaction mixture was extracted with CH2Cl2 (3×5 mL)
2. dry with materialthe combined organic extracts were dried (MgSO4)
3. concentrationconcentrated
4. customcarried on without further purification