関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Verapamil Hydrochloride | HCID 62969 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Deuterium Oxide | HCID 24602 | — |
| 生成物 | Verapamil | HCID 2520 | — |
反応手順
Verapamil hydrochloride was added to a solution of 25% deuterated sulfuric acid in deuterated water (v/v) and deuterated methanol. The solution was stirred for 140 hours at 90° C. The pH was adjusted to 12.0 and the mixture extracted with ethyl acetate. The combined ethyl acetate extracts were washed with water, dried over magnesium sulfate and evaporated to yield a viscous oil. This oil was dissolved in ether and ethereal hydrochloride was added to precipitate the hydrochloride salt. The salt was collected by filtration and crystallized from ethyl acetate to obtain deuterated verapamil as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06221335B1 |
|---|
| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-c5767c3ada7942e79ac52054414210be |
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| 出典メモ | uspto-grants-2001_04 |
|---|