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Pyridine → 4-(2-chlorophenyl)-3-(3,4-dimethoxycinnamoylamino)-1,6,8-trimethyl-2(1H)-quinolone hydrate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 3-amino-4-(2-chlorophenyl)-l,6,8-trimethyl-2(1H)quinolone | HCID 22403900 | — |
| 反応物 | 3,4-Dimethoxycinnamoylchloride | HCID 53399206 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(2-chlorophenyl)-3-(3,4-dimethoxycinnamoylamino)-1,6,8-trimethyl-2(1H)-quinolone hydrate | HCID 67770498 | 65.6% |
反応手順
A mixture of 3,4-dimethoxycinnamoyl chloride (678 mg), 3-amino-4-(2-chlorophenyl)-1,6,8-trimethyl-2(1H)-quinolone (511 mg), pyridine (0.28 ml) and THF (10 ml) was stirred at room temperature for four days. Then, the mixture was diluted with water and extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried (MgSO4). The solvent was removed and the residue was purified by a silica gel chromatography with benzene-acetone (4:1) to give crystals of 4-(2-chlorophenyl)-3-(3,4-dimethoxycinnamoylamino)-1,6,8-trimethyl-2(1H)-quinolone hydrate (510 mg, 65.6%). The crystals were recrystallized from ethanol to afford colorless prisms.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05523407 |
| 出典データセット | uspto-grants-1996_06 |
| ORD ID | ord-e83d4e6373dc467487da94c93fa7144d |
| 出典メモ | uspto-grants-1996_06 |