反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([OH:8])[CH:7]=1.I[CH:13]([CH3:15])[CH3:14].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([O:8][CH:13]([CH3:15])[CH3:14])[CH:7]=1参加物
5
実験手順
A mixture of 23 g (150 mmol) of 5-methyl-2-nitrophenol 28.1 g (1.1 x 150 mmol) of 2-iodopropane and 22.8 g (1.1 x 150 mmol) of anhydrous potassium carbonate in 150 ml of acetonitrile is stirred and refluxed for 18 hours overnight. The solids were removed, the solvent evaporated and the residue is taken up in diethyl ether and the solution washed with 50 ml of 2N potassium hydroxide (2X), brine, dried (magnesium sulfate), and evaporated to an oil. Distillation gives 18.6 g (64%) of 5-methyl-1-(1-methylethoxy)-2-nitrobenzene; bp 98°-100° C. at 0.5 mm.
後処理
- temperaturerefluxed for 18 hours overnight
- customThe solids were removed
- customthe solvent evaporated
- washthe solution washed with 50 ml of 2N potassium hydroxide (2X), brine
- dry with materialdried (magnesium sulfate)
- customevaporated to an oil
- distillationDistillation
出典と根拠
- ORDレコード
- ord-bac92b1e97c94d3db4bfaadecc55e768
- 出典データセット
- uspto-grants-1989_11
- 特許番号
- US04882357
関連ノート
読み込み中…