Dimethylcarbamoyl Chloride → 4,5-Dimethylpyridine-2-carbonitrile
반응식
[CH3:1][C:2]1[CH:3]=[N+:4]([O-])[CH:5]=[CH:6][C:7]=1[CH3:8].[CH3:10][N:11](C)C(Cl)=O.C[Si](C#N)(C)C>C(Cl)Cl>[C:10]([C:5]1[N:4]=[CH:3][C:2]([CH3:1])=[C:7]([CH3:8])[CH:6]=1)#[N:11]참가 물질
5
실험 절차
17.8 g of the obtained 3,4-dimethylpyridine-N-oxide (144.5 mmol) was dissolved under an argon gas atmosphere in 250 mL of methylene dichloride, added thereto 13.2 mL of dimethyl carbamoyl chloride (144 mmol), then 19.0 mL of trimethylsilyl cyanide (152 mmol), and stirred overnight at room temperature. The reaction solution was quenched with 10%-K2CO3 aqueous solution, the methylene dichloride layer was separated, dried on salt cake and concentrated to give 3.40 g of 6-cyano-3,4-dimethylpyridine (18% yield).
후처리
- additionadded
- customThe reaction solution was quenched with 10%-K2CO3 aqueous solution
- customthe methylene dichloride layer was separated
- customdried on salt cake
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-c7130fc8c111404c873fc7fd6081327f
- 출처 데이터셋
- uspto-grants-2015_11
- 특허 번호
- US09174906B2
반응 노트
불러오는 중…