関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | Methyl(4-aminophenoxy)acetate | HCID 6422115 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (4-Isocyanato-phenoxy)-acetic acid methyl ester | HCID 18918618 | 159.1% |
反応手順
To a mixture of (4-aminophenoxy)-acetic acid methyl ester 3 (15 g, 82.87 mmol) and triethylamine (16.77 g, 165.73 mmol) in toluene (225 ml) under nitrogen atmosphere at 0° C. was added triphosgene (9 g, 30.33 mmol) in one lot. The reaction was exo-thermic and the temperature rose to 25° C. Later the reaction mixture was heated to 75° C. over a period of one hour and maintained at this temperature for 26 hours. The reaction mixture was cooled to room temperature, the solids were filtered off, and toluene was distilled off under vacuum to get crude 4, which was vacuum distilled to get pure 4 (10 grams, 58.3%) as a white powder with an m.p between 50-53° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846845B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-3b5f043239244cea8c03e1d5a5f191d8 |
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| 出典メモ | uspto-grants-2014_09 |
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