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Water → ethyl N-[(Z)-[1-[3-nitro-4,5-bis(phenylmethoxy)phenyl]-2-[2-(trifluoromethyl)-3-pyridinyl]ethylidene]amino]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Hydrazinecarboxylic acid, ethyl ester | HCID 20064 | — |
| 反応物 | 1-(3,4-Bis(benzyloxy)-5-nitrophenyl)-2-(2-(trifluoromethyl)pyridin-3-yl)ethanone | HCID 68703897 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | ethyl N-[(Z)-[1-[3-nitro-4,5-bis(phenylmethoxy)phenyl]-2-[2-(trifluoromethyl)-3-pyridinyl]ethylidene]amino]carbamate | HCID 87588773 | — |
反応手順
A mixture of 1-(3,4-bis(benzyloxy)-5-nitrophenyl)-2-(2-(trifluoromethyl)pyridin-3-yl)ethanone (0.485 g, 0.93 mmol), ethyl carbazate (0.11 g, 1.06 mmol) and p-toluene sulfonic acid (4 mg) in toluene (10 mL) was refluxed until distillation of water ceased. The reaction mixture was cooled to room temperature, the solvents were evaporated to dryness, and the crude solid was triturated with diethyl ether (15 mL), filtered and dried yielding (Z)-ethyl 2-(1-(3,4-bis(benzyloxy)-5-nitrophenyl)-2-(2-(trifluoromethyl)pyridin-3-yl)ethylidene)-hydrazinecarboxylate, 0.475 g (84%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09446012B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-bf696df99e3c42e4bef874a61be84a2e |
| 出典メモ | uspto-grants-2016_09 |