化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Duloxetine Hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Duloxetine | HCID 60835 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Duloxetine Hydrochloride | HCID 60834 | 86% |
反応手順
Duloxetine base (99% ee, 0.5 g, 1.68 mmoles) was dissolved in acetone (5 mL) and stirred with cooling in an ice-water bath. Hydrochloric acid in diethyl ether (2M, 0.8 mL) was added, and a precipitate formed within 2 minutes. The mixture was stirred at ambient temperature 16 hours, filtered and the collected solid washed with acetone (0.5 mL). The white solid was then dried under vacuum at ambient temperature to yield duloxetine hydrochloride (0.485 g, 1.45 mmoles, yield: 86%; Chiral HPLC: 99.5% ee).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08158808B2 |
| 出典データセット | uspto-grants-2012_04 |
| ORD ID | ord-503f92caa39a48a5874a234db96d37b6 |
| 出典メモ | uspto-grants-2012_04 |