関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Methyl (2-chloroethyl)carbamate | HCID 251614 | — |
| 反応物 | 2-chloro-4-(2-2H-1,2,3-triazolylmethyl)phenol | HCID 21833677 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-[2-Chloro-4-(1-pyrazolyl)methylphenoxy]ethylcarbamic acid methyl ester | HCID 57149855 | 74.2% |
反応手順
To a mixture of potassium carbonate (435 mg), 2-chloro-4-(2-2H-1,2,3-tri-azolyl)methylphenol (300 mg) and anhydrous N,N-dimethylformamide (30 ml) was added dropwise an anhydrous N,N-dimethylformamide solution (2 ml) of 2-chloroethylcarbamic acid methyl ester (216 mg) at room temperature under stirring. This mixture was then heated at 60° C. under stirring for 6 hours, and poured into ice-cooled saturated aqueous ammonium chloride solution, which was extracted with ethyl acetate. The organic layer was washed with water and then saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel chromatography, which afforded 329 mg of 2-[2-chloro-4-(1-pyrazolyl)methylphenoxy]ethylcarbamic acid methyl ester (compound 7). Yield, 74%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05684022 |
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| 出典データセット | uspto-grants-1997_11 |
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| ORD ID | ord-7fb194e164834ab09957857f7bedc501 |
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| 出典メモ | uspto-grants-1997_11 |
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