関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Vinylidene chloride | HCID 6366 | — |
| 反応物 | 1,2-Dibromo-1-chloro-1,2,2-trifluoroethane | HCID 9634 | — |
| 反応物 | 3,4,4-Trifluoro-3-butenoic acid | HCID 15239174 | — |
| 反応物 | Ammonium persulfate sodium formate | HCID 86749473 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Cfc 113 | HCID 6428 | — |
| 生成物 | 4-Bromo-3-chloro-3,4,4-trifluorobutanoic acid | HCID 10912127 | — |
| 生成物 | 3,4-Dichloro-3,4,4-trifluorobutanoic acid | HCID 21836485 | — |
反応手順
A new method to prepare the desired 3,4,4-trifluoro-3-butenoic acid (IV) involves a one pot reaction of 1-chloro-1,2-dibromotrifluoroethane (VI) or 1,1,2-trichloretrifluoroethane (X) with vinylidene chloride in the presence of ammonium persulfate/sodium formate/air in DMF to give directly 4-bromo-3-chloro-3,4,4-trifluorobutanoic acid (VIII) or novel compound 3,4-dichloro-3,4,4-trifluoro-butanoic acid (XI). The reaction conditions to prepare XI from X are similar to those described in Hu, Chang-Ming; Qing, Feng-Ling; Zhang, Hong-Gen; J. Fluorine Chem., 1990, (49) 275-280. The formation of XI in the above reaction was confirmed by GC/MS (EI): m/z 212 (M+ 2), 210 (M+), 195, 193, 157, 155, 127, 125, 107, 105, 89, 69, 45. Dehalogenation of VIII or XI with zinc gives IV. ##STR6##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05708032 |
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| 出典データセット | uspto-grants-1998_01 |
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| ORD ID | ord-5b8186e0dd1f42ea92bb9d63f904214c |
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| 出典メモ | uspto-grants-1998_01 |
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