تفاعل #458362

معادلة التفاعل

bis-(5-chloropyrid-2-yl)ketone

trimethylsulphoxonium iodide

cetrimide

sodium hydroxide

trimethylsulphoxonium iodide

→

crude title compound

2,2-bis-(5-chloro-pyrid-2-yl)oxirane

المذيبات

water

water

1,1,1-trichloroethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated at 70° to 75° C. for 2.5 hours
2. 2
   درجة الحرارةthe mixture heated at 75° to 80° C. for a further 2 hours
3. 3
   درجة الحرارةThe mixture was cooled
4. 4
   استخلاصextracted with dichloromethane (3×20 ml)
5. 5
   تجفيفThe combined organic extracts were dried over magnesium sulfate
6. 6
   أخرىevaporated

الإجراء التجريبي

A mixture of bis-(5-chloropyrid-2-yl)ketone (0.8 g), trimethylsulphoxonium iodide (0.84 g), cetrimide (0.08 g) and sodium hydroxide (3 g) in water (16 ml) and 1,1,1-trichloroethane (30 ml) was stirred vigorously and heated at 70° to 75° C. for 2.5 hours. Further trimethylsulphoxonium iodide (0.86 g) was added and the mixture heated at 75° to 80° C. for a further 2 hours. The mixture was cooled, diluted with water (10 ml) and extracted with dichloromethane (3×20 ml). The combined organic extracts were dried over magnesium sulfate and evaporated to yield the crude title compound as a brownish paste (0.8 g), which was used directly.

المصدر