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Hydrochloric Acid → 4,4-Difluorocyclohexan-1-amine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,1-Dimethylethyl(4,4-difluorocyclohexyl)carbamate | HCID 86608981 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4,4-Difluorocyclohexan-1-amine hydrochloride | HCID 23150669 | — |
反応手順
A solution of hydrogen chloride in dioxane (4M, 1.6 ml) was added at 20° C. to a stirred solution of Intermediate 146 (140 mg, 0.6 mmol), in dioxane (1.6 ml). After 3 h, the reaction mixture was concentrated in vacuo to afford Intermediate 147 (96.5 mg) containing 4-fluoro-3-cyclohexen-1-amine. 1H NMR (400 MHz in d6-DMSO, 27° C., δ ppm) Minor component: δ8.22 (br, 3H excess), 5.18 (dm, 16 Hz, 1H), 3.28-3.13 (m, 1H excess), 2.41-1.53 (m's, 6H excess). Major component: δ8.22 (br, 3H excess), 3.28-3.13 (m, 1H excess), 2.41-1.53 (m's, 8H excess). Impurities are also present.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07528148B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-0e40c39914874464865b8c3367e3f417 |
| 出典メモ | uspto-grants-2009_05 |