참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Erlotinib Hydrochloride | HCID 176871 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Erlotinib | HCID 176870 | — |
반응 단계
The wet cake of crude erlotinib hydrochloride was added to 500 ml (10 vol.) of methanol under stirring at 25-30° C. to obtain a suspension. Sodium carbonate (33.8 g, 0.3197 mol) was added to the mixture at 25-30° C. and stirred for one hour at 25-30° C. 500 ml (10 vol.) of water was added to the reaction mixture and stirred for one hour. The crude erlotinib base was isolated by filtration and suck dried before adding it to 250 ml (5 vol.) of water at 25-30° C. and stirred for 30 min. The erlotinib base was isolated by filtration and washed with 50 ml (1 vol.) of water and suck dried to get 70 g as a wet cake. This wet cake was dried under reduced pressure at 100 mm Hg for 3 hour at 60-65° C. to afford 63 g of erlotinib base as an off-white powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09340515B2 |
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| 출처 데이터셋 | uspto-grants-2016_05 |
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| ORD ID | ord-7429b4506f93491b95fa1bc5f76707f9 |
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| 출처 메모 | uspto-grants-2016_05 |
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