関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Fluoronitrobenzene | HCID 9590 | — |
| 反応物 | 3-Chloropropanethiol | HCID 87134 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-[(3-Chloropropyl)sulfanyl]-4-nitrobenzene | HCID 14933055 | 34% |
反応手順
To a cooled (10° C.), stirred suspension of KOtBu (8.9 g, 0.080 mol) in DMSO (40 mL) was added a solution of 4-fluoronitrobenzene (11.2 g, 0.080 mol) and 3-chloropropanethiol (8.8 g, 0.080 mol) in DMSO (40 mL) over 10 minutes. The mixture was stirred at room temperature for 3.5 hours, diluted with water (1000 ml), and extracted with ether. The extracts were washed with brine, dried (MgSO4), and concentrated. Purification by flash chromatography (10% EtOAc/hexane) gave 6.2 g (34%) of product as a yellow solid m.p. 45°-48° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05104892 |
|---|
| 出典データセット | uspto-grants-1992_04 |
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| ORD ID | ord-7e3d4cb3d6324a3a900fd6ef81d27707 |
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| 出典メモ | uspto-grants-1992_04 |
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