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Potassium Carbonate → 1-Phenyl-5-(5-trifluoromethyl-thiophen-3-yloxy)-1H-tetrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1H-Tetrazole, 5-chloro-1-phenyl- | HCID 84262 | — |
| 反応物 | 4-Hydroxy-2-(trifluoromethyl)thiophene | HCID 11084273 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-Phenyl-5-(5-trifluoromethyl-thiophen-3-yloxy)-1H-tetrazole | HCID 22019466 | 68% |
反応手順
A solution of 5-trifluoromethyl-thiophen-3-ol (2.0 g, 11.9 mmol) in dry acetone (480 mL) containing 5-chloro-1-phenyl-1H-tetrazole (2.1 g, 11.9 mmol) and K2CO3 (3.3 g, 23.8 mmol) is maintained at reflux with careful exclusion of moisture overnight. The acetone is removed under reduced pressure and the residue is partitioned between CH2Cl2 (500 mL) and H2O (50 mL). The organic extracts are washed with brine, then dried (Na2SO4), filtered and concentrated. The crude product is chromatographed on silica gel, eluting with EtOAc:Hex (1:80) to afford the title compound (2.5 g, 68%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084170B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-97bd380cae1c4e708eb824535de2f9eb |
| 出典メモ | uspto-grants-2006_08 |