Ammonia → 4-Bromo-6-methylpyridin-2-amine
反応式
Br[C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[C:4]([CH3:9])[N:3]=1.[NH3:10]>>[Br:8][C:6]1[CH:5]=[C:4]([CH3:9])[N:3]=[C:2]([NH2:10])[CH:7]=1参加物
3
反応条件
- 温度
- 160 °C
実験手順
A mixture of 2,4-dibromo-6-methyl-pyridine (J. Bernstein et al., J. Amer. Chem. Soc., 1947, 69, 1147) (22.6 g, 90 mmol) and aqueous ammonia (25%, 260 ml) was stirred in an autoclave at 160° C. for 4 hr. The reaction mixture was cooled to rt and extracted with Et2O. The organic phase was dried (Na2SO4), concentrated and chromatographed (SiO2 with AcOEt/hexane/NEt3=10/30/1) to yield the title compound as a white crystalline material (4.0 g, 6%). NMR (250 MHz, DMSO): δ=3.33 (s, 3H, CH3), 6.13 (s, broad, 2H, NH2), 6.44 (s, 1H, arom-H), 6.54 (s, 1H, arom-H).
後処理
- temperatureThe reaction mixture was cooled to rt
- extractionextracted with Et2O
- dry with materialThe organic phase was dried (Na2SO4)
- concentrationconcentrated
- customchromatographed (SiO2 with AcOEt/hexane/NEt3=10/30/1)
出典と根拠
- ORDレコード
- ord-2b0dde5fa98448549c4b41a6839eda32
- 出典データセット
- uspto-grants-2004_12
- 特許番号
- US06831087B2
反応ノート
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