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Carbamic acid, ethyl ester → (9H-Xanthene-9-carbonyl)-carbamic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbamic acid, ethyl ester | HCID 5641 | — |
| 反応物 | 9H-xanthene-9-carbonyl chloride | HCID 2760892 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | (9H-Xanthene-9-carbonyl)-carbamic acid ethyl ester | HCID 9839180 | 67% |
反応手順
To a stirred solution of urethane (0.82 g, 9.21 mmol) and DMAP (0.05 g, 0.41 mmol) in pyridine (10 ml) was added at 0° C. 9H-xanthene-9-carbonyl chloride (1.50 g, 6.13 mmol). Stirring was continued at RT for 17 h, the reaction mixture was evaporated and water (50 ml)/sat. NaHCO3 solution (20 ml) was added. The solid was filtered off and crystallized from water and afterwards from EtOH/hexane to give the product (1.22 g, 67%) as a white solid, m.p. 228° C. (dec.) and MS: m/e=298.2 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06462198B1 |
| 出典データセット | uspto-grants-2002_10 |
| ORD ID | ord-a3a3fc570bf74b60a1070fa7b428c1f0 |
| 出典メモ | uspto-grants-2002_10 |