関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 7-Bromoheptanoic acid | HCID 121723 | — |
| 反応物 | Thiosemicarbazide | HCID 2723789 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 21846021 | HCID 21846021 | 96% |
反応手順
5 g of 7-bromoheptanoic acid and 2.17 g of thiosemicarbazide were introduced into 50 ml of dioxane at 90° C. and, at this temperature, 4.0 g of POCl3 were added dropwise. The mixture was then stirred at 90° C. for 1 hour. Then water was added to the mixture, and extraction 3 times with methylene chloride, drying over MgSO4 and concentration were carried out. 6.1 g (=96% yield) of product were obtained as residue.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05958923 |
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| 出典データセット | uspto-grants-1999_09 |
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| ORD ID | ord-9902cadbef08472c8438efd2e1fc0ba1 |
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| 出典メモ | uspto-grants-1999_09 |
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