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Dicyclohexylcarbodiimide → HCID 53971898、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1-Chloro-5-fluoro-4-isothiocyanato-2-[(propan-2-yl)oxy]benzene | HCID 13607933 | — |
| 反応物 | 4-Fluoro-L-proline | HCID 22214888 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 53971898 | HCID 53971898 | 89.8% |
反応手順
A mixture of 1.31 g (0.01 mol) 4-fluoroproline, 30 mL 2N KOH in methanol and 10 mL water is prepared before 2.46 g (0.01 mol) 4-chloro-2-fluoro-5-isopropoxy-phenylisothiocyanate dissolved in 250 mL methanol is added dropwise. The reaction mixture is stirred overnight at room temperature, the aqueous phase adjusted to pH 2 and the resultant product (3.77 g, See Formula X) is filtered. The compound thus obtained is dissolved in 50 mL acetonitrile before 2.59 g (0.01 mol) dicyclohexylcarbodiimide is added at room temperature. The reaction mixture is stirred for 3 h and the crude product is purified by silica gel chromatography to give 3.24 g (85% yield) of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05712225 |
| 出典データセット | uspto-grants-1998_01 |
| ORD ID | ord-804654d342e24569ad4a9a350c28f6c9 |
| 出典メモ | uspto-grants-1998_01 |