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Aniline, N-(2,2,2-trifluoroethyl)- → 6-Chloro-N-phenyl-N-(2,2,2-trifluoroethyl)pyrimidine-4-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aniline, N-(2,2,2-trifluoroethyl)- | HCID 9596 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 6-Chloropyrimidine-4-carbonyl chloride | HCID 18422098 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-Chloro-N-phenyl-N-(2,2,2-trifluoroethyl)pyrimidine-4-carboxamide | HCID 58117491 | — |
反応手順
200 mg (1.14 mmol) N-(2,2,2-trifluoroethyl)aniline and 1.14 mL (1.14 mmol) of a 1M sodium hydroxide solution were added dropwise to 212 mg (1.2 mmol) 6-chloropyrimidine-4-carboxylic acid chloride in 20 mL dichloromethane while cooling with a bath of ice and ethanol. The mixture was first stirred for 2 h with cooling and then stirred for 1 h at RT. 50 mL of a saturated sodium hydrogen carbonate solution were added and the mixture was stirred for 10 min. The organic phase was separated off, washed with water and 1M hydrochloric acid, dried on sodium sulphate, filtered and concentrated by rotary evaporation i.vac.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08110575B2 |
| 出典データセット | uspto-grants-2012_02 |
| ORD ID | ord-6c49b08b75a3495792a2a7325fc17df6 |
| 出典メモ | uspto-grants-2012_02 |