تفاعل #2439931
ord-9c4abf5b81b6451b9188e9efe6fb1ae5
معادلة التفاعل
2,7-dibromofluorenone
acetic acid
→
2,7-dibromo-9,9′-spirobifluorene
المردود 60.0%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.DISTILLATIONEther is distilled away under reduced pressure
- 2workup.ADDITIONby adding
- 3درجة الحرارةThereafter, the solution is refluxed for 1 hr
- 4ترشيحby filtering precipitate by suction
- 5غسيلby washing with water
- 6أخرىrecrystallizing with methanol
الإجراء التجريبي
According to a method similar to that of synthesis example 3, 2,7-dibromofluorenone (0.1 mol) and 2-biphenyl magnesium bromide are agitated in ether for 3 hr, followed by cooling to room temperature, further followed by slowly adding 50 ml of acetic acid. Ether is distilled away under reduced pressure, followed by adding thereto substantially 5 ml of HCl. Thereafter, the solution is refluxed for 1 hr, followed by filtering precipitate by suction, further followed by washing with water and recrystallizing with methanol. Thereby, 2,7-dibromo-9,9′-spirobifluorene is obtained (yield: 60%).