反応式
[N+:1]1([O-:19])[CH:6]=[CH:5][CH:4]=[C:3]([C:7](OC2C=CC([N+]([O-])=O)=CC=2)=[O:8])[CH:2]=1.[CH3:20][CH:21]1[CH2:26][CH2:25][CH2:24][N:23]([CH2:27][C:28]2[CH:29]=[C:30]([CH:36]=[CH:37][CH:38]=2)[O:31][CH2:32][CH2:33][CH2:34][NH2:35])[CH2:22]1>CO>[CH3:20][CH:21]1[CH2:26][CH2:25][CH2:24][N:23]([CH2:27][C:28]2[CH:29]=[C:30]([CH:36]=[CH:37][CH:38]=2)[O:31][CH2:32][CH2:33][CH2:34][NH:35][C:7]([C:3]2[CH:2]=[N+:1]([O-:19])[CH:6]=[CH:5][CH:4]=2)=[O:8])[CH2:22]1参加物
反応条件
- 温度
- 50 °C
実験手順
To the active ester thus obtained there is added a solution of 3.8 g of 3-[3-(3-methylpiperidinomethyl)phenoxy]propylamine in 70 ml of methanol and the mixture is stirred 3 hours at 50° C. The solvent is evaporated, the residue is taken up with 30 ml of N hydrochloric acid and the acid solution is washed 3 times with 20 ml of ethyl acetate. The pH is adjusted to 7.8, then the solution is salted out with sodium chloride and extracted 6 times with 30 ml of ethyl acetate. The organic extracts are collected and dried over anhydrous sodium sulfate and the solvent in evaporated to dryness. The product is purified by chromatography on silica as described in Example 7. Thus, the N-[3-[3-(3-methylpiperidinomethyl)phenoxy]propyl]-3-pyridinecarboxamide 1-oxide is obtained, identical to the product of Example 8.
後処理
- customThe solvent is evaporated
- washthe acid solution is washed 3 times with 20 ml of ethyl acetate
- extractionextracted 6 times with 30 ml of ethyl acetate
- customThe organic extracts are collected
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent in evaporated to dryness
- customThe product is purified by chromatography on silica
出典と根拠
- ORDレコード
- ord-29b42e2237774cae9ea78342356694ea
- 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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