3-Bromo-7-methyl-1-benzothiophene → 3-Cyano-7-methylbenzo[b]thiophene
반응식
Br[C:2]1[C:3]2[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:4]=2[S:5][CH:6]=1.[C:12]([Cu])#[N:13]>N1C=CC=CC=1>[C:12]([C:2]1[C:3]2[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:4]=2[S:5][CH:6]=1)#[N:13]참가 물질
4
실험 절차
3 g of 3-bromo-7-methylbenzo[b]thiophene and 1.1 g CuCN are dissolved in dry pyridine and heated at 220° in an autoclave for 12 hours. The mixture is cooled, concentrated, the residue partitioned between dichloromethane and dilute HCl and the organic phase washed, dried and concentrated. Chromatography of the residue over silica gel (toluene) yields the title compound as pale-yellow crystals. M.p.=82°-84°.
후처리
- temperatureheated at 220° in an autoclave for 12 hours
- temperatureThe mixture is cooled
- concentrationconcentrated
- customthe residue partitioned between dichloromethane and dilute HCl
- washthe organic phase washed
- customdried
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-c90280854a7b4e6fafb5bea2ad624009
- 출처 데이터셋
- uspto-grants-1988_04
- 특허 번호
- US04737516
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