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Potassium Carbonate → HCID 178418772、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Acetamidine monohydrochloride | HCID 67170 | — |
| 反応物 | Ethyl 3-(4-Fluorophenyl)-3-Oxopropanoate | HCID 2758844 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178418772 | HCID 178418772 | 87.6% |
反応手順
8.7 kg of ethyl 3-(4-fluorophenyl)-3-oxopropionate, 11.7 kg of acetoamidine hydrochloride and 28.6 kg of potassium carbonate were stirred for 5 hours at about 50° C. in 34.5 kg of methanol. Insolubles were separated from the reaction mixture and washed with methanol, and the mother liquor and the washing were combined with water and neutralized with an 18% aqueous solution of hydrochloric acid. After neutralization, the crystal was ripened by stirring under reflux for 4 hours, and the precipitated crystal was isolated by centrifugation, washed with water, dried to obtain 7.4 kg of the target compound as a white crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091206B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-87d3e58ebd044febb2246a63639c98ea |
| 出典メモ | uspto-grants-2006_08 |