참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Erlotinib | HCID 176870 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Erlotinib Hydrochloride | HCID 176871 | 90.8% |
반응 단계
Into a 3 Lt. four necked round-bottomed flask provided with a mechanical stirrer, thermometer socket, reflux condenser etc., are charged 2400 mL of methylene chloride, followed by 120 g of Erlotinib base (Prepared according to the process given in Example-(1) of PCT International Publication No. WO 2007/060691) under stirring. The reaction mass is slightly warmed up to 37±1° C., so that the Erlotinib base completely dissolves in the solvent. Then carbon treatment is given and the filtrate is transferred to 5 Lt. three necked round bottomed flask, provided with a mechanical stirrer and other accessories. To this filtrate, isopronolic HCl (HCl content as 100% is 13.90 g) is added in one lot at 30-35° C. and then the reaction mass is refluxed for about 3 hrs. Afterwards, the reaction mass is cooled to room temperature and filtered. The product is washed with methylene chloride and the wet cake is dried to get 119 g of Erlotinib hydrochloride as a white crystalline powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08748602B2 |
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| 출처 데이터셋 | uspto-grants-2014_06 |
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| ORD ID | ord-eba6c46d3da34e9cab8468e49ba6e5f0 |
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| 출처 메모 | uspto-grants-2014_06 |
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