化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Ethyl 4-{3-[3-hydroxy-4-(4-methylphenylmethoxy)benzoyl]indol-1-yl}butanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | p-Xylyl bromide | HCID 7721 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 4-[3-(3,4-dihydroxybenzoyl)indol-1-yl]butanoate | HCID 19079832 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 4-{3-[3-hydroxy-4-(4-methylphenylmethoxy)benzoyl]indol-1-yl}butanoate | HCID 19085543 | 37.9% |
反応手順
Ethyl 4-[3-(3,4-dihydroxybenzoyl)indol-1-yl]butanoate (5.70 g) was dissolved in N,N-dimethylformamide (40 ml). α-bromo-p-xylene (3.72 g) and potassium carbonate (2.57 g) were added to the resultant solution and stirred for 3 hours at room temperature. The reaction mixture was poured into 2N HCl and extracted with ethyl acetate. The resultant extract was sequentially washed with saturated sodium bicarbonate solution and brine, and then dried. The solvent was distilled off. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1), obtaining 2.77 g of ethyl 4-{3-[3-hydroxy-4-(4-methylphenylmethoxy)benzoyl]indol-1-yl}butanoate (2.77 g) as light brown crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05760040 |
| 出典データセット | uspto-grants-1998_06 |
| ORD ID | ord-b9e886295b7646c8a317bc6ffb7d90fc |
| 出典メモ | uspto-grants-1998_06 |