化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Tolperisone Hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,3-Dioxolane | HCID 12586 | — |
| 反応物 | p-Methylpropiophenone | HCID 21429 | — |
| 反応物 | Piperidine, hydrochloride (1:1) | HCID 2723721 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | Tolperisone Hydrochloride | HCID 92965 | — |
反応手順
75 kg piperidine hydrochloride and 105 kg 4-methylpropiophenone are heated to 90° C. with 180 kg of 1,3-dioxolane and 12 kg of hydrochloric acid under a nitrogen atmosphere for 7 to 20 hours. With addition of 500 kg of ethyl acetate and 440 kg MTBE at a temperature in the range of (40-80° C.), a suspension of the product is produced. After that the solid is separated from the liquid as a damp product and then dried at 60-80° C. in the vacuum oven (200-500 mbar) over a period of 12-24 hours whereby 140 kg (81.5%) of colorless crystals are isolated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07385060B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-bc1689beeb9d4730bb23488d2b6ff9ca |
| 出典メモ | uspto-grants-2008_06 |