Dimethylamine → [2-(dimethylamino)-4-pyridinyl]methanol(SALTDATA: HCl)
反応式
Cl[C:2]1[CH:7]=[C:6]([CH2:8][OH:9])[CH:5]=[CH:4][N:3]=1.[CH3:10][NH:11][CH3:12]>C(O)C>[OH:9][CH2:8][C:6]1[CH:5]=[CH:4][N:3]=[C:2]([N:11]([CH3:12])[CH3:10])[CH:7]=1参加物
4
反応条件
- 温度
- 200 °C
実験手順
A mixture of 2-chloro-4-hydroxymethylpyridine (1.0 g, 7 mmol), (prepared as described for the starting material in Example 58), and dimethylamine (30 ml of a 30% solution in ethanol) was heated in a Carius tube for 16 hours at 200° C. The mixture was allowed to cool and the mixture partitioned between saturated aqueous sodium bicarbonate solution and ethyl acetate. The organic layer was separated, dried (MgSO4) and the volatiles removed by evaporation. The residue was purified by column chromatography eluting with ethyl acetate to give 4-hydroxymethyl-2-(dimethylamino)pyridine (1 g, 94%) as a yellow oil.
後処理
- custom(prepared
- temperatureto cool
- customthe mixture partitioned between saturated aqueous sodium bicarbonate solution and ethyl acetate
- customThe organic layer was separated
- dry with materialdried (MgSO4)
- customthe volatiles removed by evaporation
- customThe residue was purified by column chromatography
- washeluting with ethyl acetate
出典と根拠
- ORDレコード
- ord-16dd58bf06ba4a15a3d44e7fb8cffe31
- 出典データセット
- uspto-grants-1999_10
- 特許番号
- US05962458
反応ノート
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