Triethylamine → 2-Ethenyl-5-nitropyridine
反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[CH:11]([B-](F)(F)F)=[CH2:12].[K+].C(N(CC)CC)C>C(O)C>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([CH:11]=[CH2:12])=[N:3][CH:4]=1)([O-:10])=[O:9]参加物
5
反応条件
- 温度
- 120 °C
実験手順
To a 20 ml, microwave tube was added 2-bromo-5-nitropyridine (0.20 g, 0.98 mmol), potassium vinyltrifluoroborate (145 mg, 1.1 mmol), PdCl2(dppf)-CH2Cl2 complex (40 mg, 0.049 mmol), and a stir bar. The tube was sealed, and ethanol (6 mL) and triethylamine (0.41 mL, 3.0 mmol) was added via syringe. The mixture was purged three times with nitrogen and then heated to 120° C. for 30 minutes. LC at that point showed mostly product. The reaction was diluted with DCM, adsorbed onto silica gel, and purified by silica gel flash chromatography (Hexane:EtOAc). LC-MS (IE, m/z): 151 [M+1]+.
後処理
- customThe tube was sealed
- customThe mixture was purged three times with nitrogen
- additionThe reaction was diluted with DCM
- custompurified by silica gel flash chromatography (Hexane:EtOAc)
出典と根拠
- ORDレコード
- ord-d3df7ab4e8044fd197f9680fa6f818f3
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09073882B2
反応ノート
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