関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 2-(4-Chlorophenyl)-4,5-dimethyl-1,3-oxazol 3-oxide | HCID 3243952 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 4-(Chloromethyl)-2-(4-chlorophenyl)-5-methyl-1,3-oxazole | HCID 3613658 | — |
反応手順
1.00 g (4.47 mmol) of the compound from Example 13A were initially charged in 15 ml of chloroform, and 1.5 ml (16.10 mmol) of phosphorus oxychloride were added carefully. With stirring, the reaction mixture was heated under reflux for 30 min. The reaction was then cooled to 0° C. and made slightly basic by addition of 25% strength aqueous ammonia solution. The mixture was extracted three times with in each case 20 ml of ethyl acetate. The combined organic phases were washed twice with in each case 5 ml of water and then dried over magnesium sulfate. The solvent was removed on a rotary evaporator. Without further purification, the residue was used for the subsequent steps.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08618119B2 |
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| 出典データセット | uspto-grants-2013_12 |
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| ORD ID | ord-962d86d60f4146a5b2ed0edd8944f1dd |
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| 出典メモ | uspto-grants-2013_12 |
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