関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Duloxetine | HCID 60835 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Duloxetine Hydrochloride | HCID 60834 | 55% |
反応手順
The free duloxetine (3 g) was first dissolved in dichloromethane (5 ml), then an ethanol solution (2 ml) containing 20% HCl was added at 0° C. with stirring, followed by hexane (40 ml). The crystalline product came out after the solution was cooled at 0-10° C. for 10 hours. The product was collected by filtration, washed with hexane and dried (1.8 g, 55% yield, m.p. 148-154° C.). Its purity was 98.4% with an optical purity of 99.6%. The DTA result shown m.p. was 160.6° C. The crystalline form, designated as Form III, was thus obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08093407B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-497e3adc26a348be81d1c3a4b7f911f4 |
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| 出典メモ | uspto-grants-2012_01 |
|---|
