1-三甲硅基吡咯烷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of methyldichlorophosphite (10.0 g, 75.24 mmol, 7.1 mL) in CH2Cl2 (50 mL) was added dropwise 1-(trimethylsilyl)pyrrolidine (13.1 mL, 10.8 g, 75.2 mmol) at 0° C. The resulting mixture was stirred for 2 h at room temperature. The solvent was removed under reduced pressure to give a colorless oil (11.97 g, 95%) as a product. 31P NMR (CDCl3) δ 182.3. The solvent was removed under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Step 1—To an ice-cold solution of pyrrolidine (167 ml, 2.00 mol) in diethyl ether (500 ml) was added a solution of chlorotrimethylsilane (127 ml, 1.00 mol) in diethyl ether (100 ml) over 1 hour. The solid was removed by filtration and washed with diethyl ether (100 ml). The filtrates were concentrated in vacuo then distilled at atmospheric pressure to give N-trimethylsilylpyrrolidine (104 g, 73%) as a colorless liquid: b.p. 139-140° C.; 1H NMR (CDCl3) 0.09 (s, 9H), 1.74 (m, 4H), 2.91 (m, 4H); 13C NMR (CDCl3) 3.50, 28.26, 48.33 The solid was removed by filtration washed with diethyl ether (100 ml) The filtrates were concentrated in vacuo then distilled at atmospheric pressure