Phosphorus oxychloride → 3-(2-Thienyl)-2-propenenitrile
反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[CH:7][C:8]([NH2:10])=O.S(S([O-])=O)([O-])(=O)=O.[Na+].[Na+].P(Cl)(Cl)(Cl)=O>O>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[CH:7][C:8]#[N:10]参加物
5
実験手順
β-(Thien-2-yl) acrylamide (5.2 g.) was mixed with sodium metabisulphite (12.9 g.) and heated with phosphoryl chloride (2.4 ml.) on a steam bath. After 1 hr., more phosphoryl chloride (10 ml.) was added and the mixture heated for a further 3.5 hrs. The mixture was cooled in an ice-bath and iced water cautiously added. The mixture was extracted into chloroform and the chloroform layer was washed with saturated sodium hydrogen carbonate solution, dried over sodium sulphate, and evaporated in vacuo to a brown oil. Distillation gave β-(thien-2 -yl) acrylonitrile, 1.50 g. (33%), b.p. 82- 86° /0.5 mm., λmax. (EtOH) 306 nm, (ε 18600).
後処理
- temperaturethe mixture heated for a further 3.5 hrs
- temperatureThe mixture was cooled in an ice-bath
- extractionThe mixture was extracted into chloroform
- washthe chloroform layer was washed with saturated sodium hydrogen carbonate solution
- dry with materialdried over sodium sulphate
- customevaporated in vacuo to a brown oil
- distillationDistillation
出典と根拠
- ORDレコード
- ord-279fc58f864a40f0ace06c9667e3d612
- 出典データセット
- uspto-grants-1977_03
- 特許番号
- US04012377
反応ノート
読み込み中…