Sodium Hydroxide → 5-Ethynyl-2,3-dimethoxypyridine
반응식
[CH3:1][O:2][C:3]1[C:8]([O:9][CH3:10])=[CH:7][C:6]([C:11]#[C:12][Si](C)(C)C)=[CH:5][N:4]=1.[OH-].[Na+]>CO>[C:11]([C:6]1[CH:7]=[C:8]([O:9][CH3:10])[C:3]([O:2][CH3:1])=[N:4][CH:5]=1)#[CH:12]참가 물질
4
실험 절차
2,3-Dimethoxy-5-[(trimethylsilyl)ethynyl]pyridine (Intermediate 31) (9.8 g, 42 mmol) was dissolved in a mixture of aqueous sodium hydroxide (21 ml, 2 M, 42 mmol) and methanol (50 ml) to give a colourless solution which was stirred for 16 hours. The reaction was evaporated and the residue was partitioned between ethyl acetate and water before the organic layer was dried and concentrated in vacuo. The crude material was purified by (SiO2; 0-10% ethyl acetate in petrol) to afford 5-ethynyl-2,3-dimethoxypyridine (5.6 g, 82%).
후처리
- customto give a colourless solution which
- customThe reaction was evaporated
- customthe residue was partitioned between ethyl acetate and water before the organic layer
- customwas dried
- concentrationconcentrated in vacuo
- customThe crude material was purified by (SiO2; 0-10% ethyl acetate in petrol)
출처 및 근거
- ORD 기록
- ord-7a477c5919c743b684e780b8f7c73222
- 출처 데이터셋
- uspto-grants-2015_11
- 특허 번호
- US09180122B2
반응 노트
불러오는 중…