Hydrazine → HCID 178507265, 화합물
반응식
[F:1][C:2]1([F:10])[CH2:4][CH:3]1[C:5](=O)[CH2:6][C:7]#[N:8].[NH2:11][NH2:12]>C(O)C>[F:1][C:2]1([F:10])[CH2:4][CH:3]1[C:5]1[CH:6]=[C:7]([NH2:8])[NH:12][N:11]=1참가 물질
4
실험 절차
Crude 3-(2,2-difluorocyclopropyl)-3-oxo-propionitrile (2 g) was dissolved in ethanol (18 mL) and treated with hydrazine (2.5 mL, 0.050 mol) at reflux for 24 hours. The reaction mixture was concentrated, diluted with brine and extracted into ethyl acetate (2×50 mL). The combined organic layers were dried (MgSO4), concentrated and purified by silica gel chromatography eluting with 1-15% methanol in methylene chloride to afford 3-(2,2-difluorocyclopropyl)-1H-pyrazol-5-amine (1.8 g, 54% yield).
후처리
- temperatureat reflux for 24 hours
- concentrationThe reaction mixture was concentrated
- additiondiluted with brine
- extractionextracted into ethyl acetate (2×50 mL)
- dry with materialThe combined organic layers were dried (MgSO4)
- concentrationconcentrated
- custompurified by silica gel chromatography
- washeluting with 1-15% methanol in methylene chloride
출처 및 근거
- ORD 기록
- ord-13bd41577a4d4e259942b8acba0ce5dc
- 출처 데이터셋
- uspto-grants-2013_03
- 특허 번호
- US08394795B2
반응 노트
불러오는 중…