関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl mercaptan | HCID 7509 | — |
| 反応物 | Benzoic acid, 3-methyl-2-nitro-, methyl ester | HCID 79621 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 2-benzylthio-3-methylbenzoate | HCID 19814653 | 77% |
反応手順
In a 5 1 pot was charged 483 g of methyl 2-nitro-3-methylbenzoate, 319 g benzyl mercaptan and 100 mL dimethyl formamide. Upon cooling to 0° C., a solution of 321 g potassium tert-butoxide in 1500 mL dimethyl formamide was added dropwise over 2.5 hours at 0°-5° C. The reaction mixture was stirred at 0° C. for 1.5 hours and then at room temperature overnight. The reaction was quenched by addition of 1 1 water and worked up by extraction with 2 1 methylene chloride. Upon washing with water (3×1 1), the methylene chloride layer was dried over MgSO4, filtered and rotovapped to give 517 g of crude methyl 2-benzylthio-3-methylbenzoate (77% yield) as a liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05157119 |
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| 出典データセット | uspto-grants-1992_10 |
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| ORD ID | ord-251b926d3d2049a88b3614d57d58e3ff |
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| 出典メモ | uspto-grants-1992_10 |
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