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Hydrochloric Acid → 7-Bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | tert-Butyl 7-bromo-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate | HCID 25220760 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 7-Bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride | HCID 66820137 | 98% |
反応手順
1,1-dimethylethyl 7-bromo-2,3-dihydro-1,4-benzoxazepine-4 (5H)-carboxylate (10 g, 30.5 mmol) was taken into hot ethanol (10 mL) followed by addition of 4M hydrogen chloride in dioxane solution (2.1 eq, 16 mL) and the resulting solution was allowed to slowly cool to ambient temperature over one hour. An excess of ethyl ether was then added and the resulting slurry was filtered. The filter cake was washed with ethyl ether and dried to give 7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride (7.9 g, 98% yield) as a colorless crystalline solid. MS (EI) for C9H10NOBr: 229 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08637499B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-3d1c6b8d66da4b39b979a793961ed21b |
| 出典メモ | uspto-grants-2014_01 |