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3,5-Dinitroaniline → 1-(3,5-Dinitrophenyl)pyrrole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,5-Dinitroaniline | HCID 12068 | — |
| 反応物 | 2,5-Dimethoxytetrahydrofuran | HCID 79098 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-(3,5-Dinitrophenyl)pyrrole | HCID 17382141 | 54% |
反応手順
A solution of 3,5-dinitroaniline (10 g, 54.644 mmol) and 2,5-dimethoxytetrahydrofuran (18.05 g, 136.61 mmol, 2.5 eq.) in acetic acid (122 ml) was heated to 100° C. for 16 h. Completion of reaction was monitored by TLC. Then the mixture was brought to RT and poured into ice-cold water. The precipitate was filtered, washed with water (150 ml) and dried to give the product in 54% yield (8.2 g). LC-MS (ESI): Calculated mass: 233.18; Observed mass: 233.04 [M+H]+ (rt: 1.667 min).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447091B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-e64e373a2f2e47dbaca16cc4542900eb |
| 出典メモ | uspto-grants-2016_09 |