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Ethanamine, 2,2,2-trifluoro- → (2',2',2'-trifluoroethyl)-6-nitro-2,2-dimethyl-2H-1-benzopyran-4-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanamine, 2,2,2-trifluoro- | HCID 9773 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 2,2'-Dipyridyl disulfide | HCID 65093 | — |
| 反応物 | 2,2-dimethyl-6-nitro-2H-1-benzopyran-4-carboxylic acid | HCID 15234744 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (2',2',2'-trifluoroethyl)-6-nitro-2,2-dimethyl-2H-1-benzopyran-4-carboxamide | HCID 131718989 | — |
反応手順
A mixture of 1.00 g of 6-nitro-2,2-dimethyl-2H-1-benzopyran-4-carboxylic acid, 0.44 g of 2,2,2-trifluoroethylamine, 0.97 g of 2,2'-dipyridyl disulfide, 1.16 g of triphenylphosphine, and 20 ml of dichloromethane was stirred at room temperature for 3 hours. The solvent was removed therefrom by distillation, and the residue was purified by silica gel column chromatography (developing solution; AcOEt:n-hexane=1:1) and then recrystallized from a mixture of n-hexane and ethyl acetate to obtain 0.98 g of N (2',2',2'-trifluoroethyl)-6-nitro-2,2-dimethyl-2H-1-benzopyran-4-carboxamide represented by formula shown below.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05412117 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-c6958f3c3a024d06824a5c716ce2de4d |
| 出典メモ | uspto-grants-1995_05 |