반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][Cl:6].[SH:7][C:8]1[N:13]2[CH:14]=[CH:15][N:16]=[C:12]2[CH:11]=[CH:10][CH:9]=1.C(N(CC)CC)C>C(O)C>[Cl:6][CH2:5][CH2:4][CH2:3][CH2:2][S:7][C:8]1[N:13]2[CH:14]=[CH:15][N:16]=[C:12]2[CH:11]=[CH:10][CH:9]=1참가 물질
5
실험 절차
In a nitrogen atmosphere, 8.87 ml (77 mmol) of 1-bromo-4-chlorobutane was added to a solution of 10.51 g (70 mmol) of 5-mercaptoimidazo[1,2-a]pyridine and 10.73 ml (77 mmol) of triethylamine in 150 ml of ethanol was added, followed by stirring at room temperature for 16 hours. After the solvent was distilled off, the residue was dissolved in dichloromethane. This solution was washed with saturated aqueous sodium hydrogen carbonate and dried, after which the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to yield 12.93 g (76.7%, light brown oily substance) of the desired product.
후처리
- additionwas added
- distillationAfter the solvent was distilled off
- dissolutionthe residue was dissolved in dichloromethane
- washThis solution was washed with saturated aqueous sodium hydrogen carbonate
- customdried
- distillationafter which the solvent was distilled off
- customThe residue was purified by column chromatography (eluent: ethyl acetate)
출처 및 근거
- ORD 기록
- ord-afc7370ad75e49a9ac250316b96f5076
- 출처 데이터셋
- uspto-grants-1998_11
- 특허 번호
- US05840732
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