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Sodium Hydroxide → N-benzyl-6-chloro-N-(2,2,2-trifluoroethyl)pyrimidine-4-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Benzyl-(2,2,2-trifluoro-ethyl)-amine | HCID 4962181 | — |
| 反応物 | 6-Chloropyrimidine-4-carbonyl chloride | HCID 18422098 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-benzyl-6-chloro-N-(2,2,2-trifluoroethyl)pyrimidine-4-carboxamide | HCID 58117522 | — |
反応手順
1.04 g (5.5 mmol) benzyl-(2,2,2-trifluoroethyl)-amine and 5.5 mL (5.5 mmol) of a 1M sodium hydroxide solution were added dropwise to 1.0 g (5.65 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 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 evaporated down 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-da8810868e5143c0aaef79dde8ed6ea1 |
| 出典メモ | uspto-grants-2012_02 |