HCID 4158166, 화합물 → 2-(Chloroethynyl)-5-nitrofuran
반응식
[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]=1참가 물질
4
실험 절차
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°.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-be08813211e54a99922aeac92e8742b8
- 출처 데이터셋
- uspto-grants-1977_05
- 특허 번호
- US04024161
반응 노트
불러오는 중…