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Formamide → 4-Fluorophenyl-tolylthiomethylformamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formamide | HCID 713 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 2-Thiocresol | HCID 8712 | — |
| 反応物 | 4-Fluorobenzaldehyde | HCID 68023 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-Fluorophenyl-tolylthiomethylformamide | HCID 86750166 | 85% |
反応手順
A solution of p-fluorobenzaldehyde (13.1 milliliters (hereinafter mL), 122 millimoles (hereinafter mmol) thiocresol (16.64 grams (hereinafter g), 122 mmol), formamide (15.0 mL, 445 mmol), and toluene (300 mL) were combined and heated to toluene reflux with azeotropic removal of H2O for 18 h. The cooled reaction was diluted with EtOAc (500 mL) and washed with satd aq Na2CO3 (3×100 mL), satd aq NaCl (100 mL), dried (Na2SO4), and concentrated. The residue was triturated with petroleum ether, filtered and dried in vacuo to afford 28.50 g of the title compound as a white solid (85%). melting point (hereinafter top)=119°-120°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05593992 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-204d0e7356d54100923539cea2134fac |
| 出典メモ | uspto-grants-1997_01 |