Chloromethyl Methyl Ether → 1-Bromo-3-(methoxymethoxy)-2-methylbenzene
反応式
[Br:1][C:2]1[C:3]([CH3:9])=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.[H-].[Na+].[CH3:12][O:13][CH2:14]Cl>CN(C)C=O>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([O:8][CH2:12][O:13][CH3:14])[C:3]=1[CH3:9]参加物
5
反応条件
- 温度
- 0 °C
実験手順
13.9 g (74 mmol) of 3-bromo-2-methylphenol are dissolved in 120 mL of dimethylformamide and the mixture is cooled to 0° C. 3.6 g (90 mmol) of 60% sodium hydride are then added portionwise and the medium is stirred for 1 hour. 6.8 mL (90 mmol) of methoxymethyl chloride are then added slowly and the medium is warmed to room temperature and then stirred for 1 hour. After the usual treatment, the residue is purified by chromatography on silica gel (eluent: 80 heptane/20 ethyl acetate). The desired product is obtained in the form of a colourless oil (m=16.2 g; Y=95%).
後処理
- temperaturethe medium is warmed to room temperature
- stirringstirred for 1 hour
- customAfter the usual treatment, the residue is purified by chromatography on silica gel (eluent: 80 heptane/20 ethyl acetate)
出典と根拠
- ORDレコード
- ord-f67322277bb34f118ca28191424cf730
- 出典データセット
- uspto-grants-2004_12
- 特許番号
- US06831106B1
反応ノート
読み込み中…