反応式
[C:1]([OH:10])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[N+:4]([O-:8])[CH:3]=1.[CH:11]1(N=C=NC2CCCCC2)CCCCC1.C[CH:27]([N:39]1[CH2:44][CH2:43][CH2:42][CH2:41][CH2:40]1)[C:28]1[CH:29]=[C:30]([CH:36]=[CH:37][CH:38]=1)[O:31][CH2:32][CH2:33][CH2:34][NH2:35]>CN(C)C1C=CN=CC=1.C(#N)C>[CH3:11][CH:43]1[CH2:42][CH2:41][CH2:40][N:39]([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:1]([C:2]2[CH:3]=[N+:4]([O-:8])[CH:5]=[CH:6][CH:7]=2)=[O:10])[CH2:44]1参加物
実験手順
To a solution of 5 g of 4-dimethylaminopyridine in 80 ml of acetonitrile there is added 5.6 g of nicotinic acid 1-oxide. The mixture is stirred 10 minutes at room temperature and then added with 9.2 g of dicyclohexylcarbodiimide. After standing 5 minutes at room temperature, there are added 10 g of 3-[3-(methylpiperidinomethyl)phenoxy]propylamine dissolved in 20 ml of acetonitrile. A weakly exothermic reaction (from 20° to 25° C.) and a dissolution which within 5 minutes is almost completed, are observed. Then the mixture is stirred 4 hours at 40° C. and the dicyclohexylurea which forms is filtered and washed with acetonitrile. After evaporation to dryness under reduced pressure, the residue 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; m.p. 108°-110° C.
後処理
- waitAfter standing 5 minutes at room temperature
- customA weakly exothermic reaction (from 20° to 25° C.)
- dissolutiona dissolution which within 5 minutes
- stirringThen the mixture is stirred 4 hours at 40° C.
- filtrationthe dicyclohexylurea which forms is filtered
- washwashed with acetonitrile
- customAfter evaporation to dryness under reduced pressure
- customthe residue is purified by chromatography on silica
出典と根拠
- ORDレコード
- ord-058b48b2507348a19f6b9a22f71dfac1
- 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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