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Acetic Anhydride → N-(3,5-dimethoxyphenyl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 3,5-Dimethoxyaniline | HCID 66301 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | N-(3,5-dimethoxyphenyl)acetamide | HCID 702039 | — |
反応手順
Acetic anhydride (13 ml, 137 mmol, 1.05 equiv) is added (in 15 min) to a suspension of 3,5-dimethoxyaniline (20 g, 131 mmol) in toluene (110 mL), keeping the internal temperature in the range of 35-45° C. The reaction mixture is allowed to stir for 20 h at RT. The resulting thick, grey suspension is diluted with hexane (55 mL) and filtered. The residue in the filter is washed with toluene/Hex (2:1, 70 mL) and Hex, and dried to provide the title compound as a white solid. API-ES-MS: 196.1 [MH]+, tR=3.03 min (purity: 100%, system 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08759517B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-b03c433ae0914093abdb6297bd798d96 |
| 出典メモ | uspto-grants-2014_06 |