関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 10-[1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarbonitrile hydrochloride | HCID 19020543 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 10-[1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxylic acid hydrochloride | HCID 14536640 | — |
反応手順
10-[(2RS)-1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarbonitrile hydrochloride (3.72 g) is added to a solution of potassium hydroxide (1.7 g) in glycol (20 cc), and the mixture is stirred for 5 hours under reflux. After cooling, the yellow solution obtained is treated with a 3N solution (10 cc) of ethereal hydrogen chloride and diluted with acetone (100 cc) and ethyl ether (100 cc), then filtered. After seeding, the yellow filtrate allows the crystallization of a product which is drained, washed with ethyl ether (2×10 cc) and dried under reduced pressure (5 mm Hg; 0.68 kPa) at 40° C. 10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxylic acid hydrochloride (3.5 g) is thereby obtained in the form of yellow crystals, m.p. 215°-217° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05321026 |
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| 出典データセット | uspto-grants-1994_06 |
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| ORD ID | ord-6918bc7a7a7844b8b6080474949de735 |
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| 出典メモ | uspto-grants-1994_06 |
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