4-Chloro-5,6-dimethylpyrimidin-2-amine → 4,5-Dimethylpyrimidin-2-amine
反応式
Cl[C:2]1[C:7]([CH3:8])=[C:6]([CH3:9])[N:5]=[C:4]([NH2:10])[N:3]=1>N.CO.[Pd]>[CH3:9][C:6]1[C:7]([CH3:8])=[CH:2][N:3]=[C:4]([NH2:10])[N:5]=1参加物
5
実験手順
A solution of 4-chloro-5,6-dimethylpyrimidin-2-amine (0.35 g, 2.22 mmol) in 2M ammonia in methanol (100 ml) was flushed with nitrogen and palladium on carbon (0.035 g, 0.33 mmol) was added, flushed with nitrogen and the reaction was hydrogenated at 1 atm, ambient temperature for 18 h. The reaction mixture was flushed with nitrogen and filtered through celite and the celite pad washed with methanol. The filtrate was evaporated to dryness in vacuo to afford 4,5-dimethylpyrimidin-2-amine (0.35 g, 2.56 mmol, 90% yield) which was used without further purification. 1H NMR (400 MHz, DMSO-d6) δ ppm 7.89 (1 H, s), 6.19 (2 H, s), 2.18 (3 H, s), 1.99 (3 H, s). MS (LC/MS) R.T.=0.56; [M+H]+=124.20.
後処理
- additionwas added
- customflushed with nitrogen
- customThe reaction mixture was flushed with nitrogen
- filtrationfiltered through celite
- washthe celite pad washed with methanol
- customThe filtrate was evaporated to dryness in vacuo
出典と根拠
- ORDレコード
- ord-a7938e16648e4662b9ef259f37665f9f
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07863291B2
反応ノート
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