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Hydrochloric Acid → Ethyl 4-chlorobenzyl[2,4-dinitro-6-(trifluoromethyl)phenyl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Benzene, 2-chloro-1,5-dinitro-3-(trifluoromethyl)- | HCID 67851 | — |
| 反応物 | Ethyl (4-chlorobenzyl)carbamate | HCID 874364 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 4-chlorobenzyl[2,4-dinitro-6-(trifluoromethyl)phenyl]carbamate | HCID 20827746 | 18% |
反応手順
Ethyl 4-chlorobenzylcarbamate (865.9 mg) and 2-chloro-3,5-dinitrobenzotrifluoride (996.7 mg) were dissolved in tetrahydrofuran (15 ml), and to the solution was added sodium hydride (162.1 mg). The reaction mixture was heated at reflux for 3 hours. After allowing to cool, to the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer-was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by silica gel column (75 g, hexane:ethyl acetate=10:1) to give the title compound (294.7 mg, 18%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06939887B2 |
| 出典データセット | uspto-grants-2005_09 |
| ORD ID | ord-b8381c3a47f54add9ea4ae9324337194 |
| 出典メモ | uspto-grants-2005_09 |