1: 3.88 g / aqueous NH3 / methanol / 24 h / cooling View Scheme

in dichloromethane T=23°C; 1.08333 h; Inert atmosphere;

in diethyl ether 2 h; Heating;

in diethyl ether 2 h; Heating;

iodine; magnesium 1.) THF, reflux, 3 h; 2.) THF, reflux, 3-5 h; Yield given. Multistep reaction;

1: 93 percent / imidazole / dimethylformamide / Ambient temperature 2: 80 percent / DIBAL / hexane; diethyl ether / 0.33 h / -78 °C 3: MgSO4 / toluene / 0 °C 4: Et3N / CH2Cl2 / Ambient temperature 5: 70 percent / HCl gas / 1) rt, overnight, 2) 60 deg C, 3 h 6: 93 percent / pyridine / CH2Cl2 / 0.17 h / 0 °C 7: 92 percent / H2 / 10percent Pd/C / ethyl acetate / 760 Torr / Ambient temperature 8: 6 M HCl / 4.5 h / 100 °C View Scheme

Yield given. Multistep reaction;

1: With recombinant Alcaligenes faecalis penicillin G acylase immobilized on oxirane acrylic carrier; potassium hydroxide in water T=35°C; pH=10; 5.33333 h; Enzymatic reaction; 2: With hydrogenchloride in water pH=1; optical yield given as percent eeenantioselective reaction;

1: LAH / tetrahydrofuran / 1 h / 0 °C 2: Et3N / CH2Cl2 / 3 h / 20 °C 3: ethanol; H2O / 12 h / 20 °C 4: BH3*Me2S / tetrahydrofuran / 3 h / 65 °C View Scheme

暂无反应条件数据