2-Chloro-3-nitropyridine → 2-Isothiocyanato-3-nitropyridine
반응식
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[N-:11]=[C:12]=[S:13].[K+]>C(O)(=O)C>[N:11]([C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1)=[C:12]=[S:13]참가 물질
4
실험 절차
A 10 g sample of 2-chloro-3-nitropyridine, an 8 g sample of potassium isothiocyanate, and 75 ml of acetic acid were combined and refluxed for 2 h. The reaction mixture was then cooled and poured into 400 ml of ice/H2O. The resulting solid was washed with water, redissolved in ethyl acetate and washed (4×) with water. The ethyl acetate solution was then treated with activated carbon, dried over anhydrous Na2SO4, filtered and evaporated to dryness to provide 3.72 g of the title compound. m.p.=115°-118° C.
후처리
- temperaturerefluxed for 2 h
- temperatureThe reaction mixture was then cooled
- washThe resulting solid was washed with water
- dissolutionredissolved in ethyl acetate
- washwashed (4×) with water
- additionThe ethyl acetate solution was then treated with activated carbon
- dry with materialdried over anhydrous Na2SO4
- filtrationfiltered
- customevaporated to dryness
출처 및 근거
- ORD 기록
- ord-f8af3a28440c4b40b27400296150885d
- 출처 데이터셋
- uspto-grants-1993_09
- 특허 번호
- US05247073
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