Potassium Carbonate → HCID 58476611、化合物
反応式
[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([C:11]#[C:12][Si](C)(C)C)=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+]>CO>[C:11]([C:5]1[CH:6]=[C:7]([N+:8]([O-:10])=[O:9])[C:2]([CH3:1])=[N:3][CH:4]=1)#[CH:12]参加物
4
実験手順
A solution of 2-methyl-3-nitro-5-[(trimethylsilyl)ethynyl]pyridine (2.32 g, 9.90 mmol) in methanol (22 mL) was cooled to 0° C. and potassium carbonate (137 mg, 0.99 mmol) was added. The reaction mixture was allowed to warm and stir at rt for 10 min, during which time a yellow precipitate formed. The reaction mixture was then concentrated and diluted with ether (200 mL). The organic solution was washed with water (200 mL) and brine (200 mL), dried over MgSO4, filtered and concentrated to give 5-ethynyl-2-methyl-3-nitropyridine (1.48 g, 92%) as a solid. LCMS (FA): Rt=1.64 min, m/z=163.0 (M+H).
後処理
- temperatureto warm
- customformed
- concentrationThe reaction mixture was then concentrated
- additiondiluted with ether (200 mL)
- washThe organic solution was washed with water (200 mL) and brine (200 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-538b316b35b3418cac9e699b243ffdb6
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07998952B2
反応ノート
読み込み中…