関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methionin AL | HCID 446793 | — |
| 反応物 | Thiourea | HCID 2723790 | — |
| 反応物 | Ethyl 3-methyl-2-(3,5-dimethylphenylacetyl)butanoate | HCID 21635576 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-(3,5-Dimethylbenzyl)-5-isopropyluracil | HCID 10730901 | 54% |
反応手順
Metal sodium (23.8 g, 1.034 mol) was reacted with anhydrous ethanol (500 ml). To the clear obtained solution, was added thiourea (54.35 g, 714 mmol) and ethyl 3-methyl-2(3,5-dimethylphenylacetyl)butanoate (13.14 g, 47.6 mol). The reaction medium was maintained under reflux for 6 h, and then was concentrated in vacuo at 40.50° C. To the obtained residue was added concentrated hydrochloric acid (100 ml) and then the solution was brought to pH 4 with acetic acid. The obtained 6-dimethylbenzyl-5-isopropyl-2-thiouracil was dissolved in an aqueous 10% chloroacetic acid solution (200 ml) and the solution was maintained under reflux for 24 h and then cooled to ambient temperature and the obtained precipitates were separated by filtration and washed with cold ethanol and then with ether, and then dried in vacuo at 40° C. to give 6-(3,5-dimethylbenzyl)-5-isopropyluracil (7 g, 54%). Melting point: 213-214° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06911450B1 |
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| 出典データセット | uspto-grants-2005_06 |
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| ORD ID | ord-cb0ad1968cf54acca043b32b31b7d52f |
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| 出典メモ | uspto-grants-2005_06 |
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