Methylamine → N,N-dimethyl-6-(methylamino)-2-Pyridinemethanamine
反応式
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][N:9]([CH3:11])[CH3:10])[N:3]=1.[CH3:12][NH2:13]>C(O)C>[CH3:10][N:9]([CH2:8][C:4]1[N:3]=[C:2]([NH:13][CH3:12])[CH:7]=[CH:6][CH:5]=1)[CH3:11]参加物
4
実験手順
2-Chloro-6-dimethylaminomethylpyridine (6.8 g, 0.04 mol), methylamine (12.0 g, 0.32 mole) and ethanol (25 ml) are heated at 180°-200° C. for 36 hours in a sealed reaction vessel. The solvent is removed in vacuo and the residue is made basic with excess sodium hydroxide and extracted with ether. The ether extract is dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. This gives 5.8 g of amber oil. The oil is distilled at 90°-100° C. at 1.8 mm and is further purified by chromatography. This gives 2.7 g of 6-dimethylaminomethyl-2-methylaminopyridine as a colorless oil.
後処理
- customThe solvent is removed in vacuo
- extractionextracted with ether
- extractionThe ether extract
- dry with materialis dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- distillationThe oil is distilled at 90°-100° C. at 1.8 mm
- customis further purified by chromatography
出典と根拠
- ORDレコード
- ord-89d8e7b7e5cd4684ada868c0ef08d323
- 出典データセット
- uspto-grants-1984_12
- 特許番号
- US04490533
反応ノート
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