化工社化工社 化学情報印刷レポート · 研究参考用
Sodium hydride → (3-(5-Chloro-2-cyano-4-fluorophenoxy)-3-(3-pyridinyl)propyl]carbamic acid 1,1 dimethylethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Chloro-2,5-difluorobenzonitrile | HCID 11275302 | — |
| 反応物 | [3-Hydroxy-3-(3-pyridinyl)propyl]carbamic acid 1,1-dimethylethyl ester | HCID 69799429 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (3-(5-Chloro-2-cyano-4-fluorophenoxy)-3-(3-pyridinyl)propyl]carbamic acid 1,1 dimethylethyl ester | HCID 86759694 | 88% |
反応手順
Sodium hydride (141 mg, 60% dispersion in oil) was added to a solution of the product from step (b) (785 mg, 2.96 mmol) and 4-chloro-2,5-difluorobenzonitrile (546 mg, 3.75 mmol) in tetrahydrofuran (9 ml) and the resultant suspension was stirred for 0.5 h. The mixture was quenched with saturated aqueous ammonium chloride, basified to pH 8 and extracted with ethyl acetate (three times). The combined organic extracts were dried (sodium sulphate), evaporated and purified by chromatography on silica eluting with petrol—acetone to give 1.05 g (88%) of the sub-title compound as a colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06887871B2 |
| 出典データセット | uspto-grants-2005_05 |
| ORD ID | ord-e90cccf4c60846e3b9d4703c2fbf62f6 |
| 出典メモ | uspto-grants-2005_05 |