HCID 86701454, 화합물 → HCID 86701455, 화합물
반응식
[CH3:1][C:2]1[C:9]([N+:10]([O-])=O)=[CH:8][C:5]([C:6]#[N:7])=[C:4]([S:13][CH3:14])[CH:3]=1.[CH:15]([Mg]Br)=[CH2:16]>C1COCC1>[CH3:1][C:2]1[C:9]2[NH:10][CH:16]=[CH:15][C:8]=2[C:5]([C:6]#[N:7])=[C:4]([S:13][CH3:14])[CH:3]=1참가 물질
4
반응 조건
- 온도
- -78 °C
실험 절차
To a solution of 4-methyl-2-(methylthio)-5-nitrobenzonitrile (1.6 g, 7.68 mmol) in THF (80 mL) at −78° C. under nitrogen, was added rapidly 1M vinylmagnesium bromide in THF (30.7 mL, 30.7 mmol). After addition was complete, the reaction was stirred at −78° C. for 30 min. The reaction was then quenched with sat. aq. NH4Cl and extracted with EtOAc. The organic extract was dried over MgSO4, filtered and concentrated. The pure title compound was isolated using FCC (0-50% EtOAc in heptanes). MS (ESI−) m/z 201.2 (M−H).
후처리
- additionAfter addition
- customThe reaction was then quenched with sat. aq. NH4Cl
- extractionextracted with EtOAc
- extractionThe organic extract
- dry with materialwas dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-0fb2a24242004d4f9406620099e63a85
- 출처 데이터셋
- uspto-grants-2015_06
- 특허 번호
- US09056874B2
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