Sodium Cyanide → 2,4-Dibromo-6-cyanomethylanisole
反応式
[Br:1][C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[C:4]([CH2:9]Br)[C:3]=1[O:11][CH3:12].[C-:13]#[N:14].[Na+]>C(O)C.O>[Br:1][C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[C:4]([CH2:9][C:13]#[N:14])[C:3]=1[O:11][CH3:12]参加物
5
実験手順
A solution of the product of stage (c) (183 g) in ethanol (150 ml) was heated to reflux. A solution of sodium cyanide (25 g) in hot water (50 ml) was added which maintained gentle refluxing. The mixture was then stirred for 5 minutes, poured into ice water, and the product was filtered off, taken up in dichloromethane, washed with water, dried over magnesium sulphate and filtered. The solvent was removed to give a brown oil which slowly crystallised. Recrystallisation from petroleum ether gave the title product as colourless needles, mp 87°-88° C.
後処理
- temperaturemaintained gentle refluxing
- filtrationthe product was filtered off
- washwashed with water
- dry with materialdried over magnesium sulphate
- filtrationfiltered
- customThe solvent was removed
- customto give a brown oil which
- customslowly crystallised
- customRecrystallisation from petroleum ether
出典と根拠
- ORDレコード
- ord-7f5418c144304f2484d21252fe552bae
- 出典データセット
- uspto-grants-1981_04
- 特許番号
- US04263037
反応ノート
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