関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,1,1-Trifluoro-2-iodoethane | HCID 67709 | — |
| 反応物 | 1,1'-Thiodi-[2-ethoxymethoxy-5-(4-trifluoromethylphenyl)benzene] | HCID 22170890 | — |
| 反応物 | Sodium Formaldehyde Sulfoxylate | HCID 23689980 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (2-Ethoxymethoxy-5-(4-trifluoromethylphenyl)phenyl] 2,2,2-trifluoroethyl sulfide | HCID 86587598 | 151.1% |
反応手順
3.3 g (5.0 mmol) of 1,1′-thiodi-[2-ethoxymethoxy-5-(4-trifluoromethylphenyl)benzene], 3.0 g (19.5 mmol) of Rongalite, 3.0 g (21.7 mmol) of potassium carbonate and 3.2 g (17.6 mmol) of 2,2,2-trifluoroethyl iodide were stirred in 50 ml of N,N-dimethylformamide at room temperature for 3 hours. The resulting reaction mixture was poured into 300 ml of water and extracted with 50 ml of ethyl acetate twice. The ethyl acetate layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 3.1 g of (2-ethoxymethoxy-5-(4-trifluoromethylphenyl)phenyl] 2,2,2-trifluoroethyl sulfide (yield 75.6%) as a pale yellow viscous liquid (nD20 1.5213).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06858639B2 |
|---|
| 出典データセット | uspto-grants-2005_02 |
|---|
| ORD ID | ord-c3157614ddee40f7b889ddcb92241301 |
|---|
| 出典メモ | uspto-grants-2005_02 |
|---|