반응 #1260705
ord-bd946f7de27e450686f890bfb8a3079f
반응 방정식
반응 조건
후처리
- 1기타In a 250 ml one-neck flask provided with a reflux condenser
- 2온도After cooling to room temperature
- 3세척The organic phase was washed with 4×50 ml of H2O
- 4건조dried over MgSO4
- 5기타the solvents were removed under reduced pressure
- 6기타The pure product was obtained by recrystallization from n-hexane
실험 절차
In a 250 ml one-neck flask provided with a reflux condenser, 990 mg (41.2 mmol) of NaH were suspended in 80 ml of dry DMF under protective gas. 10 g (30.8 mmol) of 3,6-dibromocarbazole in 80 ml of DMF were added dropwise to this reaction mixture at RT over a period of 20 minutes. A solution of 4-(tert-butyl)-benzyl bromide in 50 ml of DMF was subsequently added dropwise and the mixture was heated at 60° C. for 8 hours. After cooling to room temperature, 300 ml of water and 200 ml of ethyl acetate were carefully added. The organic phase was washed with 4×50 ml of H2O, then dried over MgSO4 and the solvents were removed under reduced pressure. The pure product was obtained by recrystallization from n-hexane. Yield: 11 g (78%); HPLC purity: 99.4%.