참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 반응물 | N-[5-bromo-6-(4-cyano-2,6-dimethylphenoxy)-2-(4-cyano-phenylamino)pyrimidin-4-yl]benzamide | HCID 70978955 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | Etravirine | HCID 193962 | — |
반응 단계
1350 ml of acetonitrile was taken into a RB flask at 27±3° C. To this was added 900 ml of IPA. To the reaction mixture 150 g of N-[5-bromo-6-(4-cyano-2,6-dimethylphenoxy)-2-(4-cyano-phenylamino)pyrimidin-4-yl]benzamide and 35.2 g of lithium hydroxide monohydrate were added and heated to 59±3° C. The reaction mixture was maintained at the same temperature for 10 hrs. After completion of the reaction, the reaction mixture was cooled to 47±3° C. and filtered. The solid was washed with acetonitrile and suck dried. The wet cake was taken into another flask to which was added 1500 ml of water, stirred for 30 mins and filtered to obtain the solid. The solid was washed with water and dried under vacuum at 73±3° C. to isolate Etravirine.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08653266B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-91e5b7c5f356461e878247d8e5899502 |
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| 출처 메모 | uspto-grants-2014_02 |
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