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1-Bromo-3-chlorobenzene → (2RS,3RS)-3-(3-chlorophenyl)-1-dimethylamino-2-methylpentan-3-ol hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Bromo-3-chlorobenzene | HCID 7928 | — |
| 反応物 | 1-(Dimethylamino)-2-methyl-3-pentanone | HCID 3048729 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 生成物 | (2RS,3RS)-3-(3-chlorophenyl)-1-dimethylamino-2-methylpentan-3-ol hydrochloride | HCID 18322695 | 19% |
反応手順
63 g of crude mixture were obtained under the conditions cited for Example 1 from 38.0 g (270 mmole) 1-dimethylamino-2-methylpentan-3-one, 74.7 g (390 mmole) 1-bromo-3-chlorobenzene and 9.50 g (390 mmole) magnesium turnings. This mixture was introduced on to a 7×45 cm column packed with silica gel and eluted with 7:1 diisopropyl ether/methanol. 12.8 g of base were obtained, from which 10.8 g of hydrochloride (4) (14% theoretical) with a melting point of 160-162° C. were obtained with trimethylchlorosilane/water in 2-butanone/ether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06248737B1 |
| 出典データセット | uspto-grants-2001_06 |
| ORD ID | ord-60742f77b0f3475c9371b8a666896567 |
| 出典メモ | uspto-grants-2001_06 |