化工社化工社 化学情報印刷レポート · 研究参考用
Pyrrolidine → 3-(3,4-dihydro-7-hydroxy-2-methyl-4-oxo-8-propyl-2H-1-benzopyran-2-yl)propanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | Methyl levulinate | HCID 69354 | — |
| 反応物 | 2',4'-Dihydroxy-3'-propylacetophenone | HCID 2775198 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-(3,4-dihydro-7-hydroxy-2-methyl-4-oxo-8-propyl-2H-1-benzopyran-2-yl)propanoic acid | HCID 13920738 | — |
反応手順
To a mixture of 20.0 g (103 mmole) of 2,4-dihydroxy-3-propylacetophenone and 15.5 g (134 mmole) of methyl levulinate in 100 ml of dry toluene was added by syringe 21.5 ml (ca. 260 mmole) of pyrrolidine. After stirring for one hour the solution was heated on a steam bath for four hours and allowed to cool. The toluene solution was washed with water and 2N NaOH. The basic solution was acidified and extracted with diethyl ether, which in turn was extracted with saturated sodium bicarbonate. The basic aqueous extract was neutralized with dilute hydrochloric acid and again extracted with diethyl ether. After drying, the solution was concentrated at reduced pressure to an oil which crystallized to the title compound, m.p. 152°-153°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04665203 |
| 出典データセット | uspto-grants-1987_05 |
| ORD ID | ord-ad21d6e5590b4931a60b1b223ce0c684 |
| 出典メモ | uspto-grants-1987_05 |