2-Chloro-3-nitropyridine → 2-Isothiocyanato-3-nitropyridine
反応式
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]参加物
4
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-f8af3a28440c4b40b27400296150885d
- 出典データセット
- uspto-grants-1993_09
- 特許番号
- US05247073
反応ノート
読み込み中…