反応式
[C:1]([OH:10])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[N+:4]([O-:8])[CH:3]=1.C(N(CC)CC)C.ClC(OCC(C)C)=O.[CH3:26][CH:27]1[CH2:32][CH2:31][CH2:30][N:29]([CH2:33][C:34]2[CH:35]=[C:36]([CH:42]=[CH:43][CH:44]=2)[O:37][CH2:38][CH2:39][CH2:40][NH2:41])[CH2:28]1>C(Cl)Cl>[CH3:26][CH:27]1[CH2:32][CH2:31][CH2:30][N:29]([CH2:33][C:34]2[CH:35]=[C:36]([CH:42]=[CH:43][CH:44]=2)[O:37][CH2:38][CH2:39][CH2:40][NH:41][C:1]([C:2]2[CH:3]=[N+:4]([O-:8])[CH:5]=[CH:6][CH:7]=2)=[O:10])[CH2:28]1参加物
実験手順
To a solution of 0.03 mol of nicotinic acid 1-oxide in 40 ml of methylene chloride containing 10 ml of triethylamine, is added, at the temperature of from 0° to 5° C. and within about 10 minutes, 0.03 mol of isobutyl chloroformate dissolved in 15 ml of methylene chloride, then the mixture is stirred 30 minutes at the same temperature. To the same mixture and at the same temperature there is added 0.03 mol of 3-[3-(3-methylpiperidinomethyl)phenoxy]propylamine dissolved in 15 ml of methylene chloride, then, after a 2 hours stirring at room temperature, the reaction mixture is washed with 10 ml of water. The organic phase is filtered, dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure. The residue is purified by chromatography on silica as described in Example 7 to yield the N-[3-[3-(3-methylpiperidinomethyl)phenoxy]propyl]-3-pyridinecarboxamide 1-oxide, identical to the product of Example 8.
後処理
- stirringafter a 2 hours stirring at room temperature
- washthe reaction mixture is washed with 10 ml of water
- filtrationThe organic phase is filtered
- dry with materialdried over anhydrous sodium sulfate
- customevaporated to dryness under reduced pressure
- customThe residue is purified by chromatography on silica
出典と根拠
- ORDレコード
- ord-e107d24521254d3c8a70e851500540a7
- 出典データセット
- uspto-grants-1985_04
- 特許番号
- US04514408
関連ノート
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