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Pyridine → (E)-N-(2,1,3-benzoxadiazol-5-ylmethoxy)-6,7-dimethoxy-3,4-dihydro-2H-naphthalen-1-imine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 3,4-Dihydro-6,7-dimethoxy-1(2H)-naphthalenone | HCID 266816 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 反応物 | (E)-6,7-dimethoxy-N-[(4-nitrophenyl)methoxy]-3,4-dihydro-2H-naphthalen-1-imine | HCID 87138450 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (E)-N-(2,1,3-benzoxadiazol-5-ylmethoxy)-6,7-dimethoxy-3,4-dihydro-2H-naphthalen-1-imine | HCID 87138747 | 88% |
反応手順
6,7-Dimethoxy-1-tetralone (40 mg, 0.19 mmol) was subjected to reaction with 0-(benzo[c][1,2,5]oxadiazol-5-ylmethyl)hydroxylamine hydrochloride (41 mg, 0.20 mmol) in ethanol (2 mL) and pyridine (0.2 mL, 2.58 mmol) under the same conditions as described for (E)-6,7-dimethoxy-3,4-dihydronaphthalen-1(2H)-one O-4-nitrobenzyl oxime. Subjection of the material obtained on work up to flash chromatography (3:7 v/v ethyl acetate/hexane elution) afforded the title compound as white crystals (60 mg, 88%), m.p. 139-140° C., Rf 0.4.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536157B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-fc6cca299ab34329b5ce188c59f8f9ed |
| 出典メモ | uspto-grants-2013_09 |