関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoyl isothiocyanate | HCID 68284 | — |
| 反応物 | Ethyl 6-Aminonicotinate | HCID 235927 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6-Thioureido-nicotinic acid ethyl ester | HCID 22019087 | 77% |
反応手順
A mixture of ethyl-6-amino-nicotinate (2.5 g, 15 mmol) and benzoyl isothiocyanate (2.45 g, 15 mmol) in THF (20 mL) was heated at 40° C. for 4 h. To this mixture at RT, was added sodium ethoxide (2.04 g, 30 mmol) in ethanol (10 mL). After stirring the resulting mixture at RT for 16 h, the volatiles were removed in vacuo. The residue was suspended in aqueous NH4Cl and the solid formed was collected by filtration, rinsed with water and dried to afford 6-thioureido-nicotinic acid ethyl ester as a white solid (2.6 g, 77% yield). LC/MS; (M+H)+=226.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07084160B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-55368fddc085434994f442da384179d4 |
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| 出典メモ | uspto-grants-2006_08 |
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