Allyl Alcohol → 2-Chloro-3-[(prop-2-en-1-yl)oxy]pyrazine
反応式
Cl[C:2]1[C:7]([Cl:8])=[N:6][CH:5]=[CH:4][N:3]=1.[CH2:9]([OH:12])[CH:10]=[CH2:11].[H-].[Na+]>CS(C)=O>[CH2:9]([O:12][C:2]1[C:7]([Cl:8])=[N:6][CH:5]=[CH:4][N:3]=1)[CH:10]=[CH2:11]参加物
5
実験手順
59.6 g of 2,3-dichloropyrazine and 92.8 g of allyl alcohol are dissolved in 400 ml of dimethylsulphoxide. 9.6 g of sodium hydride are introduced into this solution over the course of 30 minutes at 0°-5° C., whilst stirring. The mixture is then stirred for 15 hours at room temperature. Thereafter the reaction mixture is poured into 2 liters of ice water and extracted by shaking with ether. The ether extracts are washed with water, dried over sodium sulphate and evaporated in a waterpump vacuum. The residue is distilled in a high vacuum. 2-Allyloxy-3-chloro-pyrazine, boiling point 42°-44° C./0.03 mm Hg, is thus obtained.
後処理
- stirringThe mixture is then stirred for 15 hours at room temperature
- extractionextracted
- stirringby shaking with ether
- washThe ether extracts are washed with water
- dry with materialdried over sodium sulphate
- customevaporated in a waterpump vacuum
- distillationThe residue is distilled in a high vacuum
出典と根拠
- ORDレコード
- ord-65231fac7aa247708c42eb155291b10a
- 出典データセット
- uspto-grants-1983_10
- 特許番号
- US04410530
反応ノート
読み込み中…