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p-Toluenesulfonic acid → 1-(3-Dimethylaminophenyl)-2-methyl-5-phenyl-1H-pyrrole-3-carboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,3-Benzenediamine, N1,N1-dimethyl-, hydrochloride (1:2) | HCID 77124 | — |
| 反応物 | Ethyl 2-acetyl-4-oxo-4-phenylbutanoate | HCID 312893 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(3-Dimethylaminophenyl)-2-methyl-5-phenyl-1H-pyrrole-3-carboxylic acid ethyl ester | HCID 10132496 | — |
反応手順
N,N-dimethyl-1,3-phenylenediamine dihydrochloride (5 mmol, 1.0 g), triethylamine (10 mmol, 1.4 mL), 3-oxo-2-(2-oxo-2-phenyl-ethyl)-butyric acid ethyl ester (5 mmol, 1.2 g), and tosic acid (0.1 g) were combined in ethanol (25 mL), then heated under reflux (12 hrs). The solvents were removed under vacuum, the resulting oil was redissolved in methylene chloride, then applied to a silica column. The purified product was collected as a translucent oil. The named compound was identified by 1H-NMR (CDCl3, ppm): 1.28 t (3H), 2.35 s (3H), 2.77 s (6H), 4.2 q (2H), 6.3-6.7 m (4H), and 7.0-7.3 m (5H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06569890B2 |
| 出典データセット | uspto-grants-2003_05 |
| ORD ID | ord-1018c1edffcf433f8cded781d00d00c1 |
| 出典メモ | uspto-grants-2003_05 |