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Hydrochloric Acid → 1,3-Bis[4-[(3,5-dioxo-1,2,4-oxadiazolidin-2-yl)methyl]phenoxy]benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Butyloxycarbonyl isocyanate | HCID 12538171 | — |
| 反応物 | 1,3-Bis[4-(N-hydroxyaminomethyl)phenoxy]benzene | HCID 19038447 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,3-Bis[4-[(3,5-dioxo-1,2,4-oxadiazolidin-2-yl)methyl]phenoxy]benzene | HCID 19038425 | — |
反応手順
1,3-bis[4-(N-hydroxyaminomethyl)phenoxy]benzene (1.76 g) was dissolved in 35 ml of tetrahydrofuran to which, with ice-cooling and in an atmosphere of argon, was subsequently added dropwise 1.65 g of n-butoxycarbonyl isocyanate. After 30 minutes of stirring at the same temperature, 1N sodium hydroxide aqueous solution was added dropwise thereto and the stirring was continued for 30 minutes at room temperature. After adding 1N hydrochloric acid, the solvent was evaporated, and the resulting residue was subjected to silica gel column chromatography to obtain 1.0 g of 1,3-bis[4-[(3,5-dioxo-1,2,4-oxadiazolidin-2-yl)methyl]phenoxy]benzene from fractions of chloroform-methanol (30:1) elution.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05643931 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-6fe3986684ff49c8bc654087af1a8eae |
| 出典メモ | uspto-grants-1997_07 |