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(5-(3,5-Dichlorophenylthio)-1-ethyl-4-isopropyl-1H-imidazol-2-yl)methanol → HCID 69686671、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (5-(3,5-Dichlorophenylthio)-1-ethyl-4-isopropyl-1H-imidazol-2-yl)methanol | HCID 473933 | — |
| 反応物 | 2,2-Dimethylpropanecarbonyl isocyanate | HCID 12618836 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 69686671 | HCID 69686671 | 83% |
反応手順
To a solution of the compound 19 (200 mg, 0.580 mmol) in tetrahydrofuran (1 mL) under ice-cooling was added pivaloyl isocyanate (5 eq.), and stirred at the same temperature for 1 hour. After removing condenser, the reaction mixture was stirred at room temperature for 1 hour. The reaction mixture was partitioned between ethyl acetate and phosphate buffer (pH 7.0). The organic layer was separated, washed with water, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by chromatography on a silica gel column (eluate: hexane - ether (2:1)) to give the compound 81 (227 mg, 83%) as crystals. Mp. 157-159° C. Rf 0.31 (1:2 EtOAc-hexane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06054591 |
| 出典データセット | uspto-grants-2000_04 |
| ORD ID | ord-4895766e87fa4d9a921499ecd7f2a58c |
| 出典メモ | uspto-grants-2000_04 |