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Acetic Acid → alpha-(4-Benzyloxy-2-methoxyphenyl)-2-neopentylamino-5-chlorobenzyl alcohol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Pivalaldehyde | HCID 12417 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 反応物 | 2-Amino-alpha-(4-benzyloxy-2-methoxyphenyl)-5-chlorobenzyl alcohol | HCID 53931958 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | alpha-(4-Benzyloxy-2-methoxyphenyl)-2-neopentylamino-5-chlorobenzyl alcohol | HCID 54116645 | — |
反応手順
A mixture of 2-amino-α-(4-benzyloxy-2-methoxyphenyl)-5-chlorobenzyl alcohol (9.5 g), pivalaldehyde (3.35 ml), acetic acid (1.85 g) and ethanol (200 ml) was stirred for 30 min. To the mixture was added sodium cyanoborohydride (2.33 g) and the mixture was stirred for 24 h. After the mixture was concentrated in vacuo, the residue was diluted with water (200 ml) and extracted with ethyl acetate (200 ml). The extract was washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1) to give α-(4-benzyloxy-2-methoxyphenyl)-2-neopentylamino-5-chlorobenzyl alcohol (10.0 g) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726306 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-b478747f94e9498ba6d526c52d811437 |
| 出典メモ | uspto-grants-1998_03 |