関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Chlorine | HCID 24526 | — |
| 反応物 | Propyzamide | HCID 32154 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(3',5'-Dichlorophenyl)-4,4-dimethyl-5-chloro-5-dichloromethyloxazoline | HCID 54460154 | — |
反応手順
N-(1',1'-dimethylpropynyl)-3,5-dichlorobenzamide (25 gm, 0.096 m) was dissolved in methylene chloride (300 ml) and excess chlorine (2.5-3 equivalents) was bubbled through this solution at room temperature. After the starting material had disappeared (as indicated by thin layer chromatography, TLC), this solution was washed with aqueous sodium sulfite and the solvent was removed. The white solid obtained was slurried in ether (250 ml) and pyridine (8.0 gm) was added. The mixture was stirred for about 1 hour and then filtered to remove solids. The mother liquor was washed sequentially with cold 1% hydrochloric acid (25 ml), sodium bicarbonate (50 ml), water and brine. The solvent was removed after drying over magnesium sulfate and 28 gm of 2-(3',5'-dichlorophenyl)-4,4-dimethyl-5-chloro-5-dichloromethyloxazoline was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05629346 |
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| 出典データセット | uspto-grants-1997_05 |
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| ORD ID | ord-b58c25ce04724492a98d2b265a4958f1 |
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| 出典メモ | uspto-grants-1997_05 |
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