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Sulfuryl chloride → HCID 57800294、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuryl chloride | HCID 24648 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | HCID 178488085 | HCID 178488085 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 57800294 | HCID 57800294 | 80.2% |
反応手順
Sulfuryl chloride (0.39 mL, 4.86 mmol) was added dropwise to a 0° C. solution of 5-(methyloxy)-2-(trifluoromethyl)-1H-benzimidazole (1.0 g, 4.63 mmol) in HOAc (10 mL). The ice bath was removed and the mixture was allowed to stir at rt for 2 h. The concentrated reaction mixture was suspended in a mixture of EtOAc and H2O and the pH was adjusted to 7 with saturated aqueous NaHCO3. The reaction was partitioned and the aqueous portion was extracted with EtOAc. The combined organic fractions were washed with brine, dried (Na2SO4), filtered, and concentrated in vacuo to afford the title compound (0.93 g): MS (ESI) m/z 251 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08673948B2 |
| 出典データセット | uspto-grants-2014_03 |
| ORD ID | ord-e722d31834a44acd828b9010d4cfb0ce |
| 出典メモ | uspto-grants-2014_03 |