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Acetic Acid → (5-(3,5-Dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazol-2-yl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 5-(3,5-Dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazole-2-carbaldehyde | HCID 473915 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | (5-(3,5-Dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazol-2-yl)methanol | HCID 473916 | 79% |
反応手順
In 4 ml of ethanol was dissolved 440 mg (1.3 mmol)of 5-(3,5-dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazole-2-carbaldehyde (Compound I-6), followed by addition of 51 mg (1.3 mmol)of sodium borohydride at room temperature. After 10 minutes, the mixture was neutralized by acetic acid and sodium bicarbonate, and extracted with methylene chloride. The organic layer was washed with water and dried over sodium sulfate. The solvent was then concentrated under reduced pressure and the residue was recrystallized by isopropyl ether:n-hexane to provide 340 mg (yield 77%)of Compound I-8. mp 157 to 158° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05910506 |
| 出典データセット | uspto-grants-1999_06 |
| ORD ID | ord-c36273b028af494a9cab0cc5792a04aa |
| 出典メモ | uspto-grants-1999_06 |