반응식
Cl[CH2:2][C:3]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([Cl:12])[CH:10]=2)[NH:5][N:4]=1.[C-:13]#[N:14].[K+]>C(O)C.O>[C:13]([CH2:2][C:3]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([Cl:12])[CH:10]=2)[NH:5][N:4]=1)#[N:14]참가 물질
5
반응 조건
- 온도
- 5 °C
실험 절차
A solution of 3-chloromethyl-5-chloro-1H-indazole (4.5 g) in ethanol (50 ml) is dropwise added to a solution of potassium cyanide (17 g) in water (10 ml) while stirring at 5° C, and the resulting mixture is stirred at room temperature for 2 hours and at 50° C for 2 hours. The reaction mixture is cooled and the precipitated potassium chloride is removed by filtration. The filtrate is concentrated under reduced pressure, admixed with water and extracted with ether. The ether layer is washed with water, dried over anhydrous magnesium sulfate and concentrated to give 3-cyanomethyl-5-chloro-1H-indazole (3.0 g) as resinous material.
후처리
- stirringthe resulting mixture is stirred at room temperature for 2 hours and at 50° C for 2 hours
- temperatureThe reaction mixture is cooled
- customthe precipitated potassium chloride is removed by filtration
- concentrationThe filtrate is concentrated under reduced pressure
- extractionextracted with ether
- washThe ether layer is washed with water
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-b592167866d14dcd8943918814b4694a
- 출처 데이터셋
- uspto-grants-1977_02
- 특허 번호
- US04008070
연결된 노트
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