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Carbon Dioxide → 1-Benzylazetidine-3-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Disodium | HCID 141233 | — |
| 反応物 | 1-benzylazetidine-3,3-dicarboxylic Acid | HCID 11310885 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | o-Tolylacetic acid | HCID 69519 | — |
| 生成物 | 1-Benzylazetidine-3-carboxylic acid | HCID 3161318 | — |
反応手順
A mixture of the disodium salt of N-benzylazetidine-3,3-dicarboxylic acid and sodium carbonate (approximately 2:1 by weight, total weight 7.5 g) were dissolved in 100 ml of a toluene-acetic acid mixture (2/1, v/v), with immediate evolution of carbon dioxide from the sodium carbonate. The mixture was warmed and stirred, and then refluxed over a Dean and Stark water separator. After 1/2 hour evolution of carbon dioxide had ceased and 1.5 ml of an acetic acid-water mixture had separated. The slightly hazy solution was cooled to room temperature. A white fluffy solid comprising sodium acetate (3.6 ) g) was removed by filtration. Distillation of the clear filtrate yielded 4.5 g of N-benzyl-3-carboxy-azetidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04778577 |
| 出典データセット | uspto-grants-1988_10 |
| ORD ID | ord-26b063d4bc754f12a182ebb4d9486f70 |
| 出典メモ | uspto-grants-1988_10 |