関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Irinotecan acetate | HCID 131727091 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Camptosar | HCID 60837 | — |
反応手順
To a 100 mL reactor was charged amorphous irinotecan acetate (2.0 g) and methanol (14 mL). The reaction mixture was heated to 50° C. 2N hydrochloric acid (6.2 wt %, about 1.7 mL) was added to adjust the pH level to less than 4 in order to dissolve the solid particles. Ethyl acetate (40 mL) was added slowly to the mixture. The mixture was cooled to 0˜10° C. and stirred at this temperature for 1 hour. The solid particles were filtered and washed with cooled ethyl acetate (6 mL). The wet cake was dried in vacuum to give 1.66 g of irinotecan hydrochloride trihydrate Form III.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07435818B2 |
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| 出典データセット | uspto-grants-2008_10 |
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| ORD ID | ord-2aa15cc8bbfe45299c8161d26930e368 |
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| 出典メモ | uspto-grants-2008_10 |
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