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Tributylstannane → Benzopyran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tributylstannane | HCID 5948 | — |
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | 6-cyano-2,2-dimethyl-4-{1,2-dihydro-2-oxo-4-(1-phenoxythiocarbonyloxy-2-ethoxycarbonylethyl)-1-pyridinyl}-2H-benzo[b]pyran | HCID 21746910 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Benzopyran | HCID 9211 | — |
反応手順
In 3 ml of anhydrous toluene, is dissolved 73 mg of 6-cyano-2,2-dimethyl-4-{1,2-dihydro-2-oxo-4-(1-phenoxythiocarbonyloxy-2-ethoxycarbonylethyl)-1-pyridinyl}-2H-benzo[b]pyran obtained in Example 32. Then, 45 mg of 2,2'-azobisisobutyronitrile and 80 mg of tri-n-butyltin hydride are added to the solution at room temperature, and the resulting mixture is reacted at 100° C. for 30 minutes. After the reaction, the reaction mixture is directly purified by silica gel column chromatography to obtain 42 mg of 6-cyano-2,2-dimethyl-4-}-1,2-dihydro-2-oxo-4-(2-ethoxycarbonylethyl)-1pyridinyl}-2H-benzo[b]pyran.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05296492 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-d1e0c6ab5f8543d980db368112d94f4f |
| 出典メモ | uspto-grants-1994_03 |