Potassium Nitrate → HCID 23358998、化合物
反応式
[F:1][C:2]1[C:7]([F:8])=[C:6]([CH3:9])[C:5]([F:10])=[CH:4][C:3]=1[CH3:11].[N+:12]([O-])([O-:14])=[O:13].[K+]>S(=O)(=O)(O)O>[F:8][C:7]1[C:2]([F:1])=[C:3]([CH3:11])[C:4]([N+:12]([O-:14])=[O:13])=[C:5]([F:10])[C:6]=1[CH3:9]参加物
4
実験手順
To 2,3,5-trifluoro-4-methyltoluene (1.9 g) is added conc. sulfuric acid (19 ml) and the mixture is cooled to 0° C., to which a solution of potassium nitrate (1.71 g) in conc. sulfuric acid (4.6 ml) is added dropwise below 10° C. and the mixture is stirred for 15 minutes. The mixture is poured into ice-water, extracted with diethyl ether, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and the residue is purified by silica-gel column-chromatography (dichloro-methane: n-hexane=1:6) to give 2,3,6-trifluoro-4-methyl-5-nitrotoluene (1.9 g).
後処理
- additionis added dropwise below 10° C.
- extractionextracted with diethyl ether
- washthe extract is washed with water
- customdried
- distillationThe solvent is distilled off under reduced pressure
- customthe residue is purified by silica-gel column-chromatography (dichloro-methane: n-hexane=1:6)
出典と根拠
- ORDレコード
- ord-a2722392edeb4d0180fdef8f174eabf9
- 出典データセット
- uspto-grants-1997_01
- 特許番号
- US05591744
反応ノート
読み込み中…