関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N'-(2-chloroacetyl)-2,2-dimethylpropanehydrazide | HCID 54595759 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-tert-Butyl-4H-1,3,4-oxadiazin-5(6H)-one | HCID 58136344 | — |
反応手順
8.34 g (43.29 mmol) of N′-(chloroacetyl)-2,2-dimethylpropanehydrazide were dissolved in 800 ml of dry DMF, and 4.24 g (50.52 mmol) of sodium bicarbonate were added. The reaction mixture was heated at 100° C. overnight. After cooling, the solvent was removed on a rotary evaporator, water was added to the residue and the mixture was acidified with 1 N hydrochloric acid. The mixture was extracted three times with ethyl acetate, and the combined organic phases were washed with water, dried over sodium sulfate and concentrated on a rotary evaporator. This gave 5.05 g of the target compound. The crude product was reacted further without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08987256B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-271d273421ed4362b541e84fdde0b38c |
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| 出典メモ | uspto-grants-2015_03 |
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