Water → 5-Ethyl-N-methyl-2-pyridinamine
反応式
[CH2:1]([C:3]1[CH:4]=[CH:5][C:6]([NH2:9])=[N:7][CH:8]=1)[CH3:2].[Li][CH2:11]CCC.CI.O>C1COCC1>[CH2:1]([C:3]1[CH:4]=[CH:5][C:6]([NH:9][CH3:11])=[N:7][CH:8]=1)[CH3:2]参加物
6
反応条件
- 温度
- -78 °C
実験手順
A solution of 5-ethylpyridin-2-amine (330 mg, 2.70 mmol) in THF (10 mL) was cooled to −78° C. and n-BuLi (1.2 mL, 3.0 mmol) was added. The reaction stirred at −78° C. for 30 min, and then MeI (423 mg, 2.97 mmol) was added. The reaction was stirred for 2 h while warming to r.t. Water (10 mL) was added, and the solution was extracted with EtOAc (20 mL). The organic layer was dried (Na2SO4) and concentrated. The residue was purified by silica gel chromatography (PE:EtOAc=5:1) to give 35 mg (9%) of the title compound as a yellow oil. [M+H] Calc'd for C8H12N2, 137. Found, 137.
後処理
- stirringThe reaction was stirred for 2 h
- temperaturewhile warming to r.t
- extractionthe solution was extracted with EtOAc (20 mL)
- dry with materialThe organic layer was dried (Na2SO4)
- concentrationconcentrated
- customThe residue was purified by silica gel chromatography (PE:EtOAc=5:1)
出典と根拠
- ORDレコード
- ord-8fc577f8ba294c5fb402c61bb303ca11
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09242968B2
反応ノート
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