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Potassium bis(trimethylsilyl)amide → 4-Cyclopropanesulfonyl-1,2-difluoro-benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| 反応物 | 4-(3-Chloro-propane-1-sulfonyl)-1,2-difluoro-benzene | HCID 43345129 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Cyclopropanesulfonyl-1,2-difluoro-benzene | HCID 69042190 | — |
反応手順
To 11.8 mmol 4-(3-chloro-propane-1-sulfonyl)-1,2-difluoro-benzene in 400 ml THF at −78° C. was added dropwise over 30 min 14.2 mmol of a 0.9 M solution of potassium bis(trimethylsilyl)amide in THF. The reaction mixture was then allowed to warm to RT and stirring continued for a further 30 min at RT. The mixture was then quenched by addition of 1 M aq HCl and extracted three times with ethyl acetate. The combined organic phases were dried with Na2SO4, and concentrated in vacuo. The residue was chromatographed on silica gel (eluant: ethyl acetate/heptane 1:5) to afford the title compound. MS (m/e): 219.2 (M+H+, 100%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07605163B2 |
| 出典データセット | uspto-grants-2009_10 |
| ORD ID | ord-b02a159725bb4de6a2920c46ad79b85d |
| 出典メモ | uspto-grants-2009_10 |