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1-Butanol → 3'-isopropyl-3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-5'-oxazolidin-2'-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Butanol | HCID 263 | — |
| 反応物 | Dibutyl carbonate | HCID 68333 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | HCID 15557308 | HCID 15557308 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 3'-isopropyl-3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-5'-oxazolidin-2'-one | HCID 15557326 | — |
反応手順
A mixture of 3-hydroxy-3-isopropylaminomethyl-3,4-dihydro-2H-1,5-benzodioxepin (11.85 g.; 50 millimoles), prepared as described in Example 1, and dibutyl carbonate (13.1 g.) with a small piece of metallic sodium is heated in an oil bath. The temperature then is slowly raised to 170° C. with removal of butanol. Finally, the mixture is heated between 170°-200° C. with removal of excess dibutyl carbonate. The cooled reaction product is dissolved in benzene, washed with water, dried over sodium sulfate, and the solvent evaporated to give 3'-isopropyl-3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-5'-oxazolidin-2'-one, m.p. 121°-122° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03944560 |
| 出典データセット | uspto-grants-1976_03 |
| ORD ID | ord-baf10c7490ea425cbcdd0e469640b157 |
| 出典メモ | uspto-grants-1976_03 |