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Hydrochloric Acid → Ticlopidine Hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Ticlopidine | HCID 5472 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Ticlopidine Hydrochloride | HCID 65335 | — |
反応手順
Gaseous HCl (0.22 g, 0.006 mole) is bubbled into 50 ml isopropanol. The resulting solution is added dropwise to ticlopidine free base (1.5 g, 0.005 mole) in 50 ml toluene, prepared, for example as described in Example A-3, maintaining the temperature below 40° C. during the addition. The reaction mixture is stirred for 1 hour, colled to about 5°-10° C. for 1 hour, and the precipitate separated by centrifugation. An acetone slurry is made of the precipitate, brought to reflux for 1 hour, and cooled to about 5°-10° C. for 1 hour. The precipitate, ticlopidine hydrochloride (Formula IV), is separated by centrifugation, dried at 65°-70° C. under vacuum, and recrystallized from methanol. (m.p. 206.5°-207.5° C.)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04997945 |
| 出典データセット | uspto-grants-1991_03 |
| ORD ID | ord-86835d43de4841bdb7b0d898875c2034 |
| 出典メモ | uspto-grants-1991_03 |