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Hydroxyamine hydrochloride → (+/-)-trans-2-Ethyl-6-hydroxyimino-4a-(3-methoxyphenyl)-1,2,3,4,4a,5,6,7,8, 8a-decahydroisoquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | (+/-)-trans-2-Ethyl-4a-(3-methoxyphenyl)-6-oxo-1,2,3,4,4a,5,6,7,8,8a-decahydroisoquinoline hydrochloride | HCID 86752325 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (+/-)-trans-2-Ethyl-6-hydroxyimino-4a-(3-methoxyphenyl)-1,2,3,4,4a,5,6,7,8, 8a-decahydroisoquinoline | HCID 86752324 | 96.6% |
反応手順
0.5 g (1.54 mmol) of (±)-trans-2-ethyl-4a-(3-methoxyphenyl)-6-oxo-1,2,3,4,4a,5,6,7,8,8a-decahydroisoquinoline hydrochloride, 0.456 g (6.56 mmol) of hydroxylamine hydrochloride and 0.64 g of KHCO3 in 10 ml of MeOH were refluxed for 45 min. The precipitate was filtered, the solvent was removed in vacuo and the residue taken up in H2O. The pH was adjusted to 8 with conc. NH4OH, the aqueous layer was extracted with CH2Cl2. The organic layer was dried, the solvent removed in vacuo, obtaining 0.45 g of the title compound which was used as such in the subsequent step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05731322 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-4eac917dd565431a9f46b59b364b582d |
| 出典メモ | uspto-grants-1998_03 |