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Water → Acetic Acid 2-(N'-benzyloxycarbonyl-hydrazino)-2-oxo-ethyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Acetoxyacetyl chloride | HCID 26297 | — |
| 反応物 | Benzyl carbazate | HCID 79242 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Acetic Acid 2-(N'-benzyloxycarbonyl-hydrazino)-2-oxo-ethyl Ester | HCID 59796922 | — |
反応手順
To a solution of 2.04 g of hydrazine carboxylic acid benzyl ester in 40 mL of dichloromethane was added 2.57 mL of triethylamine. Under ice cooling, a solution of 1.32 mL of acetoxyacetylchloride in 20 mL of dichloromethane was added dropwise over 25 minutes, and stirred at room temperature for 1 hour. The reaction solution was added with water, extracted with ethyl acetate, and the resultant organic layer was washed with 1N hydrochloric acid, saturated aqueous sodium hydrogen carbonate and saturated brine, and then dried over magnesium sulfate. The solvent was evaporated, and the resulting solid product was washed with diethyl ether and collected by filtration, to give 1.92 g of the title compound as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429609B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-3e03aa47feeb4a069b4480543ef84765 |
| 出典メモ | uspto-grants-2008_09 |