関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 2-Amino-5-chloro-2'-fluorobenzophenone | HCID 69912 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Azido-5-chloro-2'-fluorobenzophenone | HCID 21554997 | — |
反応手順
10 G (0.04 mol) of 2-amino-5-chloro-2'-fluorobenzophenone are dissolved in a mixture of 40 ml of glacial acetic acid and 10 ml of concentrated hydrochloric acid and diazotised with 10 ml (0.04 mol) of 4 M sodium nitrite solution. The mixture is then diluted with 200 ml of ice-cold water and neutralised by addition of 16.3 g (0.12 mol) of crystalline sodium acetate. The turbid solution is clarified by filtration using active charcoal and a solution of 8.5 g (0.13 mol) of sodium azide in 100 ml of water is then added. The reaction product which has precipitated is filtered off and washed with water until neutral. After drying over potassium hydroxide/calcium chloride in a desiccator, 2-azido-5-chloro-2'-fluorobenzophenone of decomposition point 90°C is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03943145 |
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| 出典データセット | uspto-grants-1976_03 |
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| ORD ID | ord-74449a8db68b4211b700be4941ae260f |
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| 出典メモ | uspto-grants-1976_03 |
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