반응식
[CH3:1][C:2]1[O:6][C:5]2[C:7]([N+:11]([O-:13])=[O:12])=[CH:8][CH:9]=[CH:10][C:4]=2[CH:3]=1.[Cl-].[Al+3].[Cl-].[Cl-].[CH3:18][O:19]C(Cl)Cl.Cl>ClCCl>[CH:18]([C:3]1[C:4]2[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[C:5]=2[O:6][C:2]=1[CH3:1])=[O:19]참가 물질
6
실험 절차
To a mixture of 2-methyl-7-nitrobenzo[b]furan (1.77 g) and aluminum chloride (2.66 g) in dichloromethane (40 ml) was added dropwise a solution of dichloromethyl methyl ether (3.6 ml) in dichloromethane (10 ml). The mixture was stirred at ambient temperature for 30 minutes and the reaction mixture was poured into a mixture of ice and 1N-hydrochloric acid. The separated oil was extracted with dichloromethane and the extract was washed with brine, aqueous saturated sodium bicarbonate and brine. Then, the solution was dried over sodium sulfate and evaporated in vacuo. The obtained oil was crystallized from diethyl ether to give 3-formyl-2-methyl-7-nitrobenzo[b]furan (1.83 g).
후처리
- extractionThe separated oil was extracted with dichloromethane
- washthe extract was washed with brine, aqueous saturated sodium bicarbonate and brine
- dry with materialThen, the solution was dried over sodium sulfate
- customevaporated in vacuo
- customThe obtained oil was crystallized from diethyl ether
출처 및 근거
- ORD 기록
- ord-02a255bdb6784c9caf126c55bafac015
- 출처 데이터셋
- uspto-grants-1999_01
- 특허 번호
- US05858995
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