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Methane, dichloromethoxy- → 5-Trichloroacetyl-1H-pyrrole-3-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methane, dichloromethoxy- | HCID 21004 | — |
| 反応物 | 2-(Trichloroacetyl)pyrrole | HCID 321487 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane nitromethane | HCID 23431834 | — |
| 生成物 | 5-Trichloroacetyl-1H-pyrrole-3-carbaldehyde | HCID 12459977 | — |
反応手順
To a solution of the compound obtained in Step A (87 mmoles) and AlCl3 in a DCM/nitromethane mixture (80 ml/80 ml) there is added, dropwise, at −30° C., dichloro-methoxy-methane (130.5 mmoles). After stirring for two hours, the reaction mixture is poured into 800 ml of ice-cold water. The aqueous phase is extracted with AcOEt, and then the organic phases are combined. The organic phase is washed with saturated aqueous NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness to yield the title product (brown crystals), which is used directly in the next Step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541412B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-00e8b7f346ed4dddbda4d8e0c9474695 |
| 出典メモ | uspto-grants-2013_09 |