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Sodium hydride → 4-Chloro-2-[[4-(methylsulfonyl)-2-(trifluoromethyl)phenyl]thio]-benzenepropanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-Fluoro-4-(methylsulfonyl)-2-(trifluoromethyl)benzene | HCID 53415965 | — |
| 反応物 | 4-Chloro-2-mercapto-benzenepropanoic acid | HCID 67391554 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Chloro-2-[[4-(methylsulfonyl)-2-(trifluoromethyl)phenyl]thio]-benzenepropanoic acid | HCID 11669327 | — |
反応手順
Sodium hydride (60% wt. disp. oil, 0.063 g) was added to a solution of the product from step (iii) (0.180 g) in dry DMF (10 ml) and stirred at RT for 1 h before adding the product from example 44 step (i) (0.188 g). The mixture was heated at 80° C. for 1 h, then partitioned between 2M hydrochloric acid/ethyl acetate. The organics were dried, concentrated under reduced pressure to give an oil. The residue was purified by reverse phase HPLC.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08022248B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-f338bccb94e44818aa099accdb2e12a9 |
| 出典メモ | uspto-grants-2011_09 |