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Oxalic Acid → benzyl N-(2-oxoethyl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalic Acid | HCID 971 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Benzyl (2,2-dimethoxyethyl)carbamate | HCID 10800009 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | benzyl N-(2-oxoethyl)carbamate | HCID 11217768 | 50% |
反応手順
To a solution of 80 ml THF, 40 ml water, and 800 mg oxalic acid was added 9.6 g (40 mmol) of N-benzyloxycarbonyl aminoacetaldehyde dimethyl acetal, and refluxed for 4 days. The THF was removed under reduced pressure and the remaining solution was extracted with ether (3×100 ml), the ether fractions were combined and dried over anhydrous sodium sulfate. The ether was removed under reduced pressure and the remaining solution was purified by flash chromatography (hexane and ethyl acetate 3:1 then 1:1) to yield 3.88 g, 50% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05565585 |
| 出典データセット | uspto-grants-1996_10 |
| ORD ID | ord-d8425ece4df34afe83c8f585afdadcbe |
| 出典メモ | uspto-grants-1996_10 |