반응 #684663

ord-e49c7ac8abd94820ab053b8fd6da2837

반응 조건

온도
143°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04014855uspto-grants-1977_03