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Climbazole → BAY-i 9139
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Climbazole | HCID 37907 | — |
| 反応物 | Triethylammonium formate | HCID 11084032 | — |
| 生成物 | BAY-i 9139 | HCID 171440 | 56% |
反応手順
14 g (0.048 mol) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(imidazol-1-yl)-butan-2-one and 61.8 g (0.143 mol) of formic acid/triethylamine (5:2 addition compound) were heated at 145° C. for 4 hours. The reaction mixture was allowed to cool and was concentrated in vacuo. The residue was taken up in dilute sodium hydroxide solution and the mixture was extracted with methylene chloride. The organic phase was washed with water, dried over sodium sulphate and concentrated in vacuo. The residue was suspended in hot cyclohexane, the suspension was filtered hot and the solid was dried. 7.9 g (56% of theory) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(imidazol-1-yl)-butan-2-ol of melting point 145°-147° C. were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04371700 |
| 出典データセット | uspto-grants-1983_02 |
| ORD ID | ord-02f111901faa45cf844be6429bc0bf42 |
| 出典メモ | uspto-grants-1983_02 |