関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 2,5-Dimethyl-3-furanthiol | HCID 41569 | — |
| 反応物 | Triethylazanium chloride | HCID 12698378 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | O-ethyl S-(2,5-dimethyl-3-furyl) thiocarbonate | HCID 17822443 | 89.7% |
反応手順
To a mixture of ethyl chloroformate (0.86 g, 7.9 mmol) and 2,5-dimethyl-furan-3-thiol (1 g, 7.8 mmol) in methyl ethyl ketone (10 ml) was added triethylamine (0.8 g, 7.9 mmol). The mixture was cooled in ice and stirred for 3 hours. After reaching room temperature water (10 g) was added to the mixture to dissolve the triethylammonium chloride which was formed during the reaction. Concentrated hydrochloric acid (2 g) was added to neutralise the excess triethylamine. The organic layer was separated and washed with a saturated sodium hydrogen carbonate solution (10 g), water (10 g) and finally a sodium sulphate solution (10 g). After evaporation of the solvent the residue was analysed and confined by NMR spectroscopy as O-ethyl S-(2,5-dimethyl-3-furyl) thiocarbonate yield 89% (1.4 g, 7 mmol) purity 91%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06852350B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-0667694cf6c1464d972c87b8734fcae2 |
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| 出典メモ | uspto-grants-2005_02 |
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