反応式
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]([CH2:8][C:9]2[CH:10]=[C:11]([CH:17]=[CH:18][CH:19]=2)[O:12][CH2:13][CH2:14][CH2:15][NH2:16])[CH2:3]1.[C:20](O)(=[O:28])[C:21]1[CH:26]=[CH:25][CH:24]=[N+:23]([O-:27])[CH:22]=1>C(#N)C>[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]([CH2:8][C:9]2[CH:10]=[C:11]([CH:17]=[CH:18][CH:19]=2)[O:12][CH2:13][CH2:14][CH2:15][NH:16][C:20]([C:21]2[CH:22]=[N+:23]([O-:27])[CH:24]=[CH:25][CH:26]=2)=[O:28])[CH2:3]1参加物
実験手順
To a solution of 0.04 mol of 3-[3-(3-methylpiperidinomethyl)phenoxy]propylamine in 40 ml of acetonitrile, 0.04 mol of the anhydride of the nicotinic acid 1-oxide is added (Synthesis, 1981, 618), then the reaction mixture is stirred for two hours at 50°-60° C. and evaporated to dryness under reduced pressure. The residue is taken up with 20 ml of concentrated sodium hydroxide and extracted 4 times with 30 ml of ethyl acetate. The organic phase is dried over anhydrous sodium sulfate, the solvent is evaporated under reduced pressure and the product thus obtained is purified by chromatography on silica as described in Example 7. Thus, the N-[3-[3-(3-methylpiperidinomethyl)phenoxy]propyl]-3-pyridinecarboxamide 1-oxide, identical to the product of Example 8 is obtained; m.p. 108°-110° C.
後処理
- custom(Synthesis, 1981, 618)
- customevaporated to dryness under reduced pressure
- extractionextracted 4 times with 30 ml of ethyl acetate
- dry with materialThe organic phase is dried over anhydrous sodium sulfate
- customthe solvent is evaporated under reduced pressure
- customthe product thus obtained
- customis purified by chromatography on silica
出典と根拠
- ORDレコード
- ord-9ad2d2f49ff44d94882fabc184f81af7
- 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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