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Chlorosulfonic acid → 2',4'-Difluorobiphenyl-4-sulfonic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | 2,4-Difluoro-1,1'-biphenyl | HCID 169974 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2',4'-Difluorobiphenyl-4-sulfonic acid | HCID 86655179 | 40.3% |
反応手順
2,4-Difluorobiphenyl (21.2 g, 111 mmol) was dissolved in chloroform (120 mL) and chlorosulfonic acid (12.5 mL, 188 mmol) was added dropwise. The mixture was stirred overnight at room temperature. The reaction mixture was concentrated in vacuo and the residue taken up into EtOAc (100 mL) and washed with water (3×25 mL). The organics were shaken with brine, whereupon a flocculent solid formed. This was filtered and washed with EtOAc and dried to give 2′,4′-difluorobiphenyl-4-sulfonic acid as an off-white solid (12.1 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822507B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-d4c90947511b46f4b333d6a0cdd8281c |
| 出典メモ | uspto-grants-2014_09 |