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Methanol → 4-(2-Chlorophenyl)-7-ethyl-9-hydroxy-1H-[1]benzofuro[3,2-e]isoindole-1,3(2H)-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 4-(2-Chlorophenyl)-9-hydroxy-7-vinyl-1H-[1]benzofuro[3,2-e]isoindole-1,3(2H)-dione | HCID 21980708 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(2-Chlorophenyl)-7-ethyl-9-hydroxy-1H-[1]benzofuro[3,2-e]isoindole-1,3(2H)-dione | HCID 21980677 | 59% |
反応手順
A solution of (863) (0.054 g, 0.167 mmol) prepared as described in example 444 in a methanol:tetrahydrofuran mixture (1:1, 4 mL) was hydrogenated over Raney nickel (100 mg) and hydrogen. The product was purified by column chromatography using a gradient of 0–100% ethyl acetate in dichloromethane to give (864) (0.032 g, 59%). 1H NMR δ [(CD3)2SO] 9.65 (s, 1H), 7.92 (m, 1H), 7.56 (d, J=3.0 Hz, 1H), 7.43 (m, 3H), 6.96 (d, J=2.5 Hz, 1H), 2.90 (q, 2H), 1.5 (t, 3H). MH−:392, 390.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094798B1 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-62cae9a2d35848e7979fc9f2cc564996 |
| 出典メモ | uspto-grants-2006_08 |