化工社化工社 化学情報印刷レポート · 研究参考用
Hydrogen chloride-ethyl acetate → 8-(1-Cyclohexylethoxy)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| 反応物 | tert-butyl 8-(1-cyclohexylethoxy)-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate | HCID 68429333 | — |
| 生成物 | 8-(1-Cyclohexylethoxy)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine hydrochloride | HCID 68429491 | 79% |
反応手順
A mixture of the compound obtained in step 1 (0.47 g) and 4N hydrogen chloride/ethyl acetate (3 mL) was stirred at room temperature for 3 hr. The precipitate was collected by filtration, and recrystallized from ethanol-diisopropyl ether to give the title compound (0.31 g, 79%) as a white powder. 1H-NMR (DMSO-d6): δ0.85-1.30 (5H, m), 1.18 (3H, t, J=6.2 Hz), 1.45-1.85 (6H, m), 3.56 (2H, brs), 4.24-4.32 (4H, m), 4.84-5.00 (1H, m), 6.55 (1H, d, J=8.1 Hz), 7.75 (1H, d, J=8.1 Hz), 9.56 (2H, brs)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08329687B2 |
| 出典データセット | uspto-grants-2012_12 |
| ORD ID | ord-c52132d8f0a54e808d54d3668af37405 |
| 出典メモ | uspto-grants-2012_12 |