Phosphorus pentachloride → HCID 59180425、化合物
反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11](O)(=[O:13])=[O:12])=[C:7]([I:15])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].P(Cl)(Cl)(Cl)(Cl)[Cl:17]>ClC(Cl)C>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([Cl:17])(=[O:13])=[O:12])=[C:7]([I:15])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2]参加物
4
反応条件
- 温度
- 77.5 °C
実験手順
To a suspension of 100 (12.0 g; 35.0 mmol) in dichloroethane (300 mL) at 50° C. was added phosphorus pentachloride (11.01 g; 52.9 mmol). After addition was complete, the reaction mixture was heated at 75-80° C. overnight, cooled to 50° C., and additional phosphorus pentachloride (6.0 g; 28.8 mmol) was added. After heating at 85° C. for an additional 12 hours, the reaction mixture was again cooled to 50° C. and additional phosphorus pentachloride (2.0 g; 9.60 mmol) was added. Heating was continued at 90° C. for 4 hours, cooled to room temperature, and concentrated under reduced pressure. The resulting crude oil was purified by automated silica gel column chromatography (Biotage®) eluting with ethyl acetate/hexanes (0 to 20% v/v over 400 mL gradient elution) to give the title compound as a yellow oil (9.98 g).