反应详情

温度

0 °C

To a solution of carbonothioate 80 (1.29 g, 3.93 mmol) in ice-cold CH2Cl2 (20 mL) was added sulfuryl chloride (478 μL, 5.89 mmol) and the mixture was stirred at 0° C. for 2 h 35 min, after which the mixture was concentrated to dryness, providing chloroformate 81 as a colorless gum (1.44 g, >quant.) which was used directly in the next step: 1H NMR (400 MHz, CDCl3) δ 1.33 (t, J=7.1 Hz, 6H), 2.05-2.14 (m, 2H), 2.68-2.75 (m, 2H), 4.07-4.15 (m, 4H), 5.84 (s, 2H): 31P NMR (162 MHz, CDCl3) δ 30.08 (s).

1. concentrationafter which the mixture was concentrated to dryness