반응식
C1C(=O)N([Cl:8])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.[Cl:27][C:28]1[C:33]([C:34]#[N:35])=[CH:32][CH:31]=[C:30]([CH3:36])[N:29]=1>C1C=CC=CC=1>[Cl:27][C:28]1[C:33]([C:34]#[N:35])=[CH:32][CH:31]=[C:30]([CH2:36][Cl:8])[N:29]=1참가 물질
5
실험 절차
NCS (1.44 g, 10.8 mmol) and benzoyl peroxide (238 mg, 0.98 mmol) were added to a stirred solution of 2-chloro-3-cyano-6-methyl-pyridine (750 mg, 4.92 mmol) in benzene (35 mL) and the mixture was heated to reflux. After 4 h, the mixture was cooled and filtered. The filtrate was diluted with ethyl acetate and was washed with sodium metabisulfite solution, water and brine, dried (Na2SO4) and evaporated in vacuo. The residue was purified by chromatography on silica (chloroform) to give the title compound:
후처리
- temperaturethe mixture was heated to reflux
- temperaturethe mixture was cooled
- filtrationfiltered
- additionThe filtrate was diluted with ethyl acetate
- washwas washed with sodium metabisulfite solution, water and brine
- dry with materialdried (Na2SO4)
- customevaporated in vacuo
- customThe residue was purified by chromatography on silica (chloroform)
출처 및 근거
- ORD 기록
- ord-770e2c5221a6477481db72971c6ebf26
- 출처 데이터셋
- uspto-grants-2002_04
- 특허 번호
- US06376499B1
연결된 노트
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