関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | O,O-diethyl phosphorochloridothioate | HCID 17305 | — |
| 反応物 | 5-(Ethylsulfanyl)-3-hydroxythiophene-2-carbonitrile | HCID 21317930 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Cyano-3-(diethoxythiophosphoryloxy)-5-ethylthio-thiophene | HCID 53827054 | 86.8% |
反応手順
7 g of potassium carbonate and 9.4 g of O,O-diethyl chlorothiophosphate were added to a solution of 9.3 g of 2-cyano-3-hydroxy-5-ethylthio-thiophene in 150 ml of acetonitrile and the mixture was stirred for 24 hours at 20° C. and was filtered. The filtrate was evaporated to dryness and the residue was chromatographed over silica gel. Elution with an 8-2 cyclohexane-ethyl acetate mixture yielded 14.6 g of 2-cyano-3-(diethoxythiophosphoryloxy)-5-ethylthio-thiophene with a refractive index of nD20 = 1.5635.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04128562 |
|---|
| 出典データセット | uspto-grants-1978_12 |
|---|
| ORD ID | ord-e62d9c3939ae42bf9f760fd70880f123 |
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| 出典メモ | uspto-grants-1978_12 |
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