반응식
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]#[N:7].[N-:8]=[N+:9]=[N-:10].[Na+].[Cl-].[Al+3].[Cl-].[Cl-].Cl>O1CCCC1.CCCCC>[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]1[NH:10][N:9]=[N:8][N:7]=1참가 물질
7
반응 조건
- 온도
- 80 °C
실험 절차
100mmol of 5-chlorovaleronitrile are placed under an inert atmosphere in 100 ml of anhydrous tetrahydrofuran on an ice bath. 445 mmol of sodium azide and then 100 mmol of aluminum chloride are then added in small fractions. The reaction mixture is heated to 80° C. and left under reflux, with stirring, for 16 hours. The complex formed is then hydrolyzed by addition, dropwise, of 150 cm3 of 5% hydrochloric acid. The resulting aqueous phase is extracted with ethyl acetate and after washing the organic phase with water, then with a saturated sodium chloride solution, drying and evaporation, the residue obtained is taken up in pentane. The expected product is then obtained after filtration of the precipitate formed.
후처리
- waitleft
- temperatureunder reflux
- customThe complex formed
- additionis then hydrolyzed by addition
- extractionThe resulting aqueous phase is extracted with ethyl acetate
- washafter washing the organic phase with water
- dry with materialwith a saturated sodium chloride solution, drying
- customevaporation
- customthe residue obtained
출처 및 근거
- ORD 기록
- ord-7c5079c0fe654c1b83febdf8eee3497c
- 출처 데이터셋
- uspto-grants-1996_10
- 특허 번호
- US05561113
연결된 노트
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