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 34A is initially charged in 15 ml of chloroform, and 1.5 ml (16.10 mmol) of phosphoryl chloride are added carefully. With stirring, the reaction mixture is heated at reflux for 30 min. The mixture is then cooled to 0° C. and made weakly basic by addition of aqueous ammonia. The mixture is extracted three times with in each case 20 ml of ethyl acetate. The combined organic phases are washed twice with in each case 5 ml of water and then dried over magnesium sulphate. The solvent is removed on a rotary evaporator. Without further purification, the product obtained in this manner is used for the subsequent reactions.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08653109B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-25949300d859422d843e2576b5adf79a |
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| 出典メモ | uspto-grants-2014_02 |
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