Methylamine → N,N-dimethyl-6-(methylamino)-2-Pyridinemethanamine
반응식
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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-89d8e7b7e5cd4684ada868c0ef08d323
- 출처 데이터셋
- uspto-grants-1984_12
- 특허 번호
- US04490533
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