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Sodium hydride → 4-Chloro-6-(2,2,2-trifluoro-1-phenyl-ethoxy)-pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4,6-Dichloropyrimidine | HCID 70943 | — |
| 反応物 | (S)-alpha-(Trifluoromethyl)benzyl alcohol | HCID 95556 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-Chloro-6-(2,2,2-trifluoro-1-phenyl-ethoxy)-pyrimidine | HCID 86614301 | 95% |
反応手順
NaH (60%, 120 mg, 3.0 mmol) was added to a solution of 2,2,2-trifluoro-1-phenyl-ethanol (350 mg, 2.03 mmol) in 5 ml of THF. The mixture was stirred for 20 minutes at room temperature. 4,6-Dichloro-pyrimidine (300 mg, 2.03 mmol) was added and then the reaction mixture was heated at 70° C. for 1 hour. After cooling, the THF was evaporated to provide a residue, which was dissolved in 15 ml of EtOAc, and then washed with water, and dried over sodium sulfate. The solvent was removed by rotovap to give 550 mg of 4-chloro-6-(2,2,2-trifluoro-1-phenyl-ethoxy)-pyrimidine, yield 95%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08093291B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-6ea2c035d77d4d45b80fd7302edf29aa |
| 出典メモ | uspto-grants-2012_01 |