関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Dimethyl phosphorochloridothionate | HCID 17304 | — |
| 反応物 | 5-Pyrimidinol, 2-(1,1-dimethylethyl)- | HCID 163499 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | O,O-dimethyl O-(2-(1,1-dimethylethyl)-5-pyrimidinyl) phosphorothioate | HCID 13277768 | — |
反応手順
To a stirred mixture of 6 grams of 2-(1,1-dimethylethyl)-5-pyrimidinol, 6 grams of finely powdered potassium carbonate and 40 ml of acetonitrile was added 6.33 grams of O,O-dimethyl phosphorochloridothioate. The mixture was stirred without external heating until all O,O-dimethyl phosphorochloridothioate was consumed as shown by GLC. The solids present were removed by filtration, the filtrate concentrated under vacuum, the residue taken up in diethyl ether, the ether solution washed twice with 2% aqueous sodium hydroxide, once with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was removed under vacuum, while leaving a pale amber colored oil having a refractive index at 25° of 1.5027. Elemental analysis showed the product to contain 43.82% carbon; 6.09% hydrogen and 10.10% nitrogen. Theoretical composition is 43.47% carbon; 6.20% hydrogen and 10.14% nitrogen.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04429125 |
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| 出典データセット | uspto-grants-1984_01 |
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| ORD ID | ord-79b16d3355814f209b9d0f23520e8982 |
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| 出典メモ | uspto-grants-1984_01 |
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