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Nitric Acid → Diclopentezol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | (2R)-2-amino-1-phenylpropan-1-ol;hydrochloride | HCID 198220 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 1-(2,4-Dichlorophenyl)-2-(1,2,4-triazol-1-yl)-4,4-dimethyl1-penten-3-one | HCID 54030782 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | Diclopentezol | HCID 91738 | 100.3% |
反応手順
To d-norephedrine hydrochloride (832 g) and monochlorobenzene (2,343 g), a dimethylformamide solution of sodium borohydride (166 g) was added, and the resultant mixture was stirred at a temperature of 20° to 30° C. for 1 hour. A monochlorobenzene solution of the E isomer of 1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-4,4-dimethyl1-penten-3-one (991 g) was added thereto, followed by stirring at the same temperature as above for 10 hours. The reaction mixture was treated with dilute nitric acid. The monochlorobenzene layer was separated and concentrated to give the E isomer of 1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-4,4-dimethyl-1-penten-3-ol (1,000 g) (content, 97.0%; yield, 97.0%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04904793 |
| 出典データセット | uspto-grants-1990_02 |
| ORD ID | ord-13c346453b1344d8b00b96497f1e5aa2 |
| 出典メモ | uspto-grants-1990_02 |