関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Maleic Acid | HCID 444266 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 1-[1-(4-Chlorophenyl)cyclobutyl]-3-hydroxy-3-methylbutan-1-one oxime | HCID 86743936 | — |
| 触媒 | Molybdic acid | HCID 82208 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 4-Amino-4-[1-(4-chlorophenyl)cyclobutyl]-2-methylbutan-2-ol maleate | HCID 67945541 | — |
反応手順
A solution of 1-[1-(4-chlorophenyl)cyclobutyl]-3-hydroxy-3-methylbutan-1-one oxime (2 g) in methanol (70 ml) was cooled to -10° C. and molybdic acid (1.67 g) added with stirring. Sodium borohydride (2.7 g) was added portionwise. The temperature of the reaction mixture was maintained at 0° C. for 21/2 hours and then water (200 ml) was added. The reaction mixture was extracted with ether, the extract filtered, and the filtrate washed with water and dried. Removal of the solvents yielded an oil which was dissolved in ether. A solution of maleic acid in ether was added and a gum was formed which solidified to give 4-amino-4-[1-(4-chlorophenyl)cyclobutyl]-2-methylbutan-2-ol maleate (m.p. 139°-144° C. (dec)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05047432 |
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| 出典データセット | uspto-grants-1991_09 |
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| ORD ID | ord-f60cd1d7155c459eab08064226917a22 |
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| 出典メモ | uspto-grants-1991_09 |
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