反应详情

温度

90 °C

Formaldehyde (0.954 g, 31.8 mmole, 1.2 eq. 37% WT in water), Dimethylphosphane oxide (2.25 g, 28.8 mmole, 1.09 eq.) and tert-butyl piperazine-1-carboxylate (14.93 g, 26.5 mmole, 1.0 eq.) were dissolved in 20 mL of anhydrous ethyl alcohol. The reaction mixture was sealed in a seal-tube with N2 atmosphere and stirred at 90 Celsius overnight. The reaction mixture was then cooled to room temperature and rotaevaporate to remove volatile components. The light yellow thick oil obtained was purified via column chromatography (elution sequence: 100% hexane-10% EtOAc/hexane-100% EtOAc-10% MeOH/EtOAc/sat.NH3) to yield 1.01 g of the desired compound as white solid. MS (LC/MS): 299.2 [M+Na]

1. temperatureThe reaction mixture was then cooled to room temperature
2. customto remove volatile components
3. customThe light yellow thick oil obtained
4. customwas purified via column chromatography (elution sequence: 100% hexane-10% EtOAc/hexane-100% EtOAc-10% MeOH/EtOAc/sat.NH3)