Sodium Azide → 1-(Azidomethyl)cyclopropanecarbonitrile
반응식
CS(O[CH2:6][C:7]1([C:10]#[N:11])[CH2:9][CH2:8]1)(=O)=O.[N-:12]=[N+:13]=[N-:14].[Na+]>CN(C)C=O.O.C(OCC)(=O)C.CCOCC>[N:12]([CH2:6][C:7]1([C:10]#[N:11])[CH2:9][CH2:8]1)=[N+:13]=[N-:14]참가 물질
7
반응 조건
- 온도
- 120 °C
실험 절차
A stirred mixture of (1-cyanocyclopropyl)methyl methanesulfonate (21.52 mmol, 3.77 g) and sodium azide (43.0 mmol, 2.80 g) in N,N-dimethyl formamide (40 mL) was heated to 120° C. for ˜18 hours. The mixture was allowed to cool and was diluted with water and ethyl acetate. The organic layer was separated, dried over sodium sulphate and concentrated under reduced pressure to give an oil. This oil was taken up in ether and washed with water, dried and concentrated under reduced pressure to give the intermediate 1-(azidomethyl)cyclopropanecarbonitrile (1.8 g) as an oil.
후처리
- temperatureto cool
- customThe organic layer was separated
- dry with materialdried over sodium sulphate
- concentrationconcentrated under reduced pressure
- customto give an oil
- washwashed with water
- customdried
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-5597d936b6ae4680a161d3e6251e8fdc
- 출처 데이터셋
- uspto-grants-2014_06
- 특허 번호
- US08759352B2
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