Methylamine → 2-Chloro-4-(methylamino)-5-nitrobenzonitrile
반응식
[CH3:1][NH2:2].[Cl:3][C:4]1[CH:11]=[C:10](F)[C:9]([N+:13]([O-:15])=[O:14])=[CH:8][C:5]=1[C:6]#[N:7]>C1COCC1>[Cl:3][C:4]1[CH:11]=[C:10]([NH:2][CH3:1])[C:9]([N+:13]([O-:15])=[O:14])=[CH:8][C:5]=1[C:6]#[N:7]참가 물질
4
반응 조건
- 온도
- -20 °C
실험 절차
A solution of MeNH2 in THF (14.9 mL, 2 M, 29.8 mmol) was added dropwise to a solution of 2-chloro-4-fluoro-5-nitrobenzonitrile (3.0 g, 15 mmol) in THF (100 mL) at −20° C. The mixture was stirred at −20° C. for 1 h and thereafter concentrated, washed with brine and extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. The resulting residue was washed with PE to give the sub-title compound.
후처리
- concentrationconcentrated
- washwashed with brine
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- washThe resulting residue was washed with PE
출처 및 근거
- ORD 기록
- ord-f1119eec4ec94833850b30c3926a1f5a
- 출처 데이터셋
- uspto-grants-2013_06
- 특허 번호
- US08466186B2
반응 노트
불러오는 중…