反応式
COC[N:4]1[CH:8]=[CH:7][N:6]=[C:5]1[C:9]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=1)[OH:10].C(O)(=O)C.Cl>O>[C:21]1([C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=2)([C:5]2[NH:4][CH:8]=[CH:7][N:6]=2)[OH:10])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1参加物
実験手順
A mixture of 13 g. (0.037 mol) of 1-methoxymethyl-α-phenyl-α-(m-trifluoromethyl-phenyl)imidazole-2-methanol, 100 ml. of glacial acetic acid, 10 ml. of concentrated hydrochloric acid and 10 ml. of water was refluxed for three hours. After cooling, the liquid was distilled off and the residue was dissolved in a small amount of ethanol. The solution was made alkaline with 2 N sodium hydroxide solution and the alcohol was evaporated. The remaining aqueous phase was then extracted with diethyl ether. The extract was dried over sodium sulphate and the ether was distilled off. The residue was crystallised from toluene, the toluenic solution being decolorised with active charcoal. There was obtained α-phenyl-α-(m-trifluoromethyl-phenyl)imidazole-2-methanol. Melting point 151.5°-152.5° C.
後処理
- additionA mixture of 13 g
- temperatureAfter cooling
- distillationthe liquid was distilled off
- dissolutionthe residue was dissolved in a small amount of ethanol
- customthe alcohol was evaporated
- extractionThe remaining aqueous phase was then extracted with diethyl ether
- dry with materialThe extract was dried over sodium sulphate
- distillationthe ether was distilled off
- customThe residue was crystallised from toluene
出典と根拠
- ORDレコード
- ord-13c164782d4d4c179c9b278d8ad5d032
- 出典データセット
- uspto-grants-1979_05
- 特許番号
- US04152441
関連ノート
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