反应详情

温度

143 °C

A mixture of pentabromophenol (100 g., 0.2 moles), potassium carbonate (30 g., 0.22 moles), potassium iodide (0.5 g.), dimethyl formamide (180 ml.) and 3,3-bischloromethyl oxetane (15.5 g., 0.1 moles) was stirred in a nitrogen atmosphere and heated to 143° C. for 5 hours. The partially cooled reaction mixture was poured into 1 liter of water. The resulting solid 3,3-bis[pentabromophenoxymethyl]oxetane was collected by filtration and washed on the funnel with water and with ethanol. The yield was 93 g. A small sample was recrystallized from a large volume of dioxane. The recrystallized material melted at 281°-284° C.

1. customThe partially cooled reaction mixture
2. filtrationThe resulting solid 3,3-bis[pentabromophenoxymethyl]oxetane was collected by filtration
3. washwashed on the funnel with water and with ethanol
4. customA small sample was recrystallized from a large volume of dioxane