참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | 5-Fluoro-1-(2-fluorobenzyl)-3-iodo-1H-pyrazolo[3,4-b]pyridine | HCID 58065602 | — |
| 반응물 | HCID 178418260 | HCID 178418260 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-Fluoro-1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carbonitrile | HCID 56846743 | — |
반응 단계
A suspension of 16.03 g (43.19 mmol) of 5-fluoro-1-(2-fluorobenzyl)-3-iodo-1H-pyrazolo[3,4-b]pyridine (Example 6A) and 4.25 g (47.51 mmol) of copper cyanide was initially charged in DMSO (120 ml) and stirred at 150° C. for 2 h. After cooling, the contents of the flask were cooled to about 40° C. and poured into a solution of conc. aqueous ammonia (90 ml) and water (500 ml), ethyl acetate (200 ml) was added and the mixture was subjected to brief extractive stirring. The aqueous phase was separated off and extracted two more times with ethyl acetate (200 ml each time). The combined organic phases were washed twice with 10% strength aqueous sodium chloride solution (100 ml each time), dried and concentrated under reduced pressure. The crude product was reacted without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08921377B2 |
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| 출처 데이터셋 | uspto-grants-2014_12 |
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| ORD ID | ord-712014c1a8854c18a4ffd5d5e55b3170 |
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| 출처 메모 | uspto-grants-2014_12 |
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