化工社化工社 化学情報印刷レポート · 研究参考用
Resorcinol → 1,2-Dihydro-9-hydroxy-1-methyl-7-(3-methyl-2-octyl)-4-oxo4H-thieno-[2,3-c][1] benzopyran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Resorcinol | HCID 5054 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 5-(3-Methyloctan-2-yl)benzene-1,3-diol | HCID 258176 | — |
| 反応物 | Methyl tetrahydro-4-methyl-3-oxo-2-thiophenecarboxylate | HCID 10487456 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 1,2-Dihydro-9-hydroxy-1-methyl-7-(3-methyl-2-octyl)-4-oxo4H-thieno-[2,3-c][1] benzopyran | HCID 21519990 | — |
反応手順
A solution in dry benzene of equimolar amounts of methyl 4-methyl-3-oxo-tetrahydrothiophene-2-carboxylate and 5-(3-methyl-2-octyl) resorcinol plus phosphorous oxychloride (5 ml. of benzene/g. of the resorcinol) was warmed for 13 days at 35°-37°C. in an oil bath. Most of the benzene and HCl were removed at reduced pressure, and the dark tarry residue was stirred with ether and water until solution was complete. The ether layer was washed successively with dilute solutions of sodium bicarbonate, sodium hydroxide and sodium carbonate, then with water and saturated sodium chloride. Drying and concentrating the final organic solution left a friable brick-red foamy solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03946111 |
| 出典データセット | uspto-grants-1976_03 |
| ORD ID | ord-a079d58fdd594ec28413d3cb891bd874 |
| 出典メモ | uspto-grants-1976_03 |