関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 2-Methoxy-5-nitroaniline | HCID 7447 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Acetamide, N-(2-methoxy-5-nitrophenyl)- | HCID 97239 | — |
反応手順
504 g (3 mol) of 2-amino-4-nitro-1-methoxybenzene are introduced into 860 ml of acetic acid and 600 ml of water (or the combined main filtrate and first wash filtrate of a previous batch) and the mixture is heated to 80° C. 358 g (3.2 mol) of acetic anhydride are added dropwise in the course of 10 minutes. The mixture is subsequently stirred at 80° C. for 4 hours, and then cooled to room temperature, while stirring, by removing the heating bath and finally to 15° C. The pale yellow needles which have precipitated are filtered off with suction, washed with 300 ml of 60% strength acetic acid and 1500 ml of water in several portions and dried.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05387716 |
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| 出典データセット | uspto-grants-1995_02 |
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| ORD ID | ord-81e010c1cada4efabc4550a7a913a1fe |
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| 出典メモ | uspto-grants-1995_02 |
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