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Sulfuric Acid → (1,3-Dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | N-Phthaloylglycine | HCID 20825 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | (1,3-Dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid butyl ester | HCID 357739 | 194.4% |
反応手順
A mixture of 160 ml of butanol, 20.0 g of (1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid (94.6 mmol) and 2.0 ml of concentrated sulfuric acid was refluxed with stirring for 24 h. Then 5 g of sodium bicarbonate were added in portions, stirring continued at r.t. for 5 min and the solvent evaporated in vacuo. The residue was partitioned between 100 ml of water and 100 ml of ethyl acetate. The organic phase was washed with 100 ml of brine, dried over sodium sulfate and was evaporated in vacuo to give a yellowish oil that later solidified. 24.02 g of the title compound were obtained; MS-(+)-ion: M+1=261.9.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09339527B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-3a8864168ff345fbacafb690c8825395 |
| 出典メモ | uspto-grants-2016_05 |