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Pyridine → (8E)-8-(2,1,3-benzoxadiazol-5-ylmethoxyimino)-3-methoxy-6,7-dihydro-5H-naphthalen-2-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 7-Hydroxy-6-methoxy-1-tetralone | HCID 316840 | — |
| 反応物 | O-(benzo[c][1,2,5]oxadiazol-5-ylmethyl)hydroxylamine hydrochloride | HCID 66760966 | — |
| 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 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | (8E)-8-(2,1,3-benzoxadiazol-5-ylmethoxyimino)-3-methoxy-6,7-dihydro-5H-naphthalen-2-ol | HCID 87138555 | 9% |
反応手順
7-Hydroxy-6-methoxy-1-tetralone (83 mg, 0.43 mmol) was subjected to reaction with O-(benzo[c][1,2,5]oxadiazol-5-ylmethyl)hydroxylamine hydrochloride (96 mg, 0.48 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 off-white crystals (13 mg, 9%), m.p. 138° C. (with decomposition), 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-68ac811b29fb4c24bcd874146743570d |
| 出典メモ | uspto-grants-2013_09 |