化工社化工社 化学情報印刷レポート · 研究参考用
Water → 3-[(6-Methoxy-4-chromanylidene)amino]-2-oxazolidinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 6-methoxy-3,4-dihydro-2H-1-benzopyran-4-one | HCID 4612168 | — |
| 反応物 | 3-amino-1,3-oxazolidin-2-id-4-one | HCID 178514269 | — |
| 触媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 3-[(6-Methoxy-4-chromanylidene)amino]-2-oxazolidinone | HCID 70615282 | — |
反応手順
A solution of 62 g (0.61 mole) of 3-amino-2-oxazolidone in 650 ml of benzene was treated with 15 drops of HCl (isopropanol) solution using mechanical stirring, and refluxed until all water was removed via a Dean-Stark trap. The solution was then treated with 107 g (0.60 mole) of 6-methoxy-4-chromanone and refluxed for 11.5 hr. A 9.6 ml portion of water (theory: 10.8 ml) was collected. The reaction mixture was stripped of benzene under the water pump. The residue was taken up in 200 ml of 1:1 isopropanol:ether, stored 24 hr at room temperature, refrigerated overnight and filtered. The resultant cream-colored solid was washed with 125 ml of isopropanol, ether, and dried. M.p. 54°-64°; yield: 115 g (73%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04093627 |
| 出典データセット | uspto-grants-1978_06 |
| ORD ID | ord-a2a0b1b410ce48e0bda49330495e0e76 |
| 出典メモ | uspto-grants-1978_06 |