HCID 4158166、化合物 → 2-(Chloroethynyl)-5-nitrofuran
反応式
[Cl:1][C:2](Cl)=[CH:3][C:4]1[O:5][C:6]([N+:9]([O-:11])=[O:10])=[CH:7][CH:8]=1.CC(C)([O-])C.[K+]>C(O)(C)(C)C>[Cl:1][C:2]#[C:3][C:4]1[O:5][C:6]([N+:9]([O-:11])=[O:10])=[CH:7][CH:8]=1参加物
4
実験手順
To a stirred solution of 20.8 g of 1 in 100 ml of dry tert-butanol was added dropwise at 5°-10° over a 30-minute period a solution of 11.2 g of potassium tert-butoxide in 100 ml of tert-butanol. The mixture then was stirred at 5°-10° for 1 hour longer. Concentration of the mixture under reduced pressure gave a dark residue which was extracted with ether and water. The ether phase was separated, dried over magnesium sulfate and Claisen distilled to give 4 as a liquid, b.p.: 73°-76° at 0.2 torr which solidified on standing, the solid having a melting point of 38°-41°.
後処理
- customConcentration of the mixture under reduced pressure gave a dark residue which
- extractionwas extracted with ether and water
- customThe ether phase was separated
- dry with materialdried over magnesium sulfate and Claisen
- distillationdistilled
出典と根拠
- ORDレコード
- ord-be08813211e54a99922aeac92e8742b8
- 出典データセット
- uspto-grants-1977_05
- 特許番号
- US04024161
反応ノート
読み込み中…