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Hydrochloric Acid → Ethyl 3-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 3-chlorobenzylcarbamate | HCID 17071127 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 3-chlorobenzyl[2,4-dinitro-6-(trifluoromethyl)phenyl]carbamate | HCID 20827739 | 9.4% |
反応手順
Ethyl 3-chlorobenzylcarbamate (720.3 mg) and 2-chloro-3,5-dinitrobenzotrifluoride (829.1 mg) were dissolved in tetrahydrofuran (20 ml), and to the solution was added sodium hydride (147.1 mg). The reaction mixture was heated at reflux for 1.5 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 (129.5 mg, 9%).
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-65ef8bcd7f7e4b638673690370d62ffb |
| 出典メモ | uspto-grants-2005_09 |