関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Erlotinib | HCID 176870 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Erlotinib Hydrochloride | HCID 176871 | 84.2% |
反応手順
Into a 2 Lt. four necked round-bottomed flask provided with a mechanical stirrer, thermometer socket, reflux condenser etc., are charged 1340 mL of methanol, followed by Erlotinib base 60 g. (Prepared according to the process given in Example-(1) of PCT International Publication No. WO 2007/060691). The reaction mass is warmed to around 40° C. so that Erlotinib base completely dissolves. To this reaction mass, carbon treatment is given and the filtrate is transferred to another 2 Lt. four necked flask. To this solution isopropanolic HCl (HCl content as 100% is 6.12 g) is added in one lot and the reaction mass is stirred at 30-35° C. for about 90 minutes and filtered. The product is washed with fresh methanol and dried the wet cake to get 55.2 g of Erlotinib hydrochloride as a white crystalline powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08748602B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-9106fa1dbe6e4bf3b36718b48813247e |
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| 出典メモ | uspto-grants-2014_06 |
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