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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 | 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 (5.50 mmol) benzyl-(2,2,2-trifluorethyl)-amine and 5.50 mL (5.50 mmol) of a 1M sodium hydroxide solution were added dropwise while cooling with a bath of ice/ethanol to 1.00 g (5.65 mmol) 6-chloropyrimidine-4-carboxylic acid chloride in 20 mL dichloromethane. The mixture was first stirred for 2 h while being cooled and then for a further 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 (1×30 mL) and 1M hydrochloric acid (1×50 mL), dried on sodium sulphate, filtered and evaporated down i. vac. The product was reacted further without any further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829006B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-85f255f912d74627b1b16b998fbcf446 |
| 出典メモ | uspto-grants-2014_09 |