関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phosphorochloridic acid, dimethyl ester | HCID 101863 | — |
| 反応物 | 5-Butoxy-3-hydroxythiophene-2-carbonitrile | HCID 21317900 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-Butoxy-2-cyanothiophen-3-yl dimethyl phosphate | HCID 21317904 | 76.8% |
反応手順
7.7 g of potassium carbonate and 7.7 g of O,O-dimethyl chlorophosphate were added to a solution of 11 g of 2-cyano-3-hydroxy-5-n-butoxy-thiophene in 150 ml of acetonitrile and the mixture was stirred for 16 hours at 20° C. and was filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was dissolved in ether. The ether solution was washed with water containing 100 g/l of sodium chloride and then with 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride. The ether phase was dried and treated with activated carbon, filtered and concentrated to dryness to obtain 12.5 g of 2-cyano-3-(dimethoxyphosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.511.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04128562 |
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| 出典データセット | uspto-grants-1978_12 |
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| ORD ID | ord-432cda9a55fc428fafdceacba2e3aaea |
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| 出典メモ | uspto-grants-1978_12 |
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