Bromine → 9-Bromomethyl-6,11-dihydro-11-oxodibenz[b,e]oxepin
반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][O:10][C:9]3[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=3[C:7](=[O:16])[C:6]=2[CH:17]=1.[Br:18]Br>BrCCBr.[W]>[Br:18][CH2:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][O:10][C:9]3[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=3[C:7](=[O:16])[C:6]=2[CH:17]=1참가 물질
5
실험 절차
To a stirred and irradiated (Tungsten lamp) solution of 2.0 gm of the 9-methyl compound of Step B in 5 ml of 1,2-dibromoethane, add a solution of 1.7 gm of bromine in 5 ml of 1,2-dibromoethane dropwise over a period of 1 hour at 150° C. Cool the reaction mixture, pour into ice water and extract with water and dry over sodium sulfate. Concentrate to dryness and crystallize the residue from isopropyl ether to obtain the title product.
후처리
- temperatureCool the reaction mixture
- extractionextract with water
- dry with materialdry over sodium sulfate
- concentrationConcentrate to dryness
- customcrystallize the residue from isopropyl ether
출처 및 근거
- ORD 기록
- ord-e89b81fa23844afb95cbe6a582941ca0
- 출처 데이터셋
- uspto-grants-1981_08
- 특허 번호
- US04282365
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