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Phthalic Acid → tert-Butyl 1-oxa-6-azaspiro(2.5)octane-6-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phthalic Acid | HCID 1017 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-Boc-4-Methylenepiperidine | HCID 2756808 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | tert-Butyl 1-oxa-6-azaspiro(2.5)octane-6-carboxylate | HCID 22135564 | 83.6% |
反応手順
13.5 g of tert-butyl 4-methylene-1-piperidinecarboxylate was dissolved in 300 ml methanol, and 28.3 g phthalic acid monoperacid magnesium salt and 8.62 g sodium bicarbonate were added thereto, and the mixture was stirred at room temperature for 1 day. The reaction solution was filtered through Celite, and the resulting filtrate was evaporated. Ethyl acetate was added to the resulting residue which was then washed with water and brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was evaporated, and subjected to silica gel column chromatography to give 12.2 g of tert-butyl 1-oxa-6-azaspiro[2.5]octane-6-carboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06699870B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-88932765c1a24248bf34df8e7ab3a97d |
| 出典メモ | uspto-grants-2004_03 |