참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Nitrogen | HCID 947 | — |
| 반응물 | 2-Chloro-1,3-bis(dimethylamino)trimethinium hexafluorophosphate | HCID 10590807 | — |
| 반응물 | HCID 178509245 | HCID 178509245 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 3-Bromo-6-chloropyrazolo[1,5-a]pyrimidine | HCID 67346936 | 80.8% |
반응 단계
A 5 L 4-neck round bottom flask equipped with mechanical stirrer, thermocouple, condenser and N2 bubbler was charged with 3-amino-4-bromopyrazole (40.0 g, 240 mmol), 2-Chloro-1,3-bis(dimethylamino)trimethinium hexafluorophosphate (77.0 g, 252 mmol) in acetic acid (390 ml)/ethanol (580 ml). The reaction mixture was heated to 70° C. for 8 hrs. Cool to 0° C. Filter off solids. Wash solids with 500 ml water then 500 ml MeOH and dried under high vac to afford the title compound (45.1 g, 194 mmol). LRMS (APCI) calc'd for (C6H3BrClN3) [M+H]+, 231.9; found 231.9. 1H NMR (CDCl3, 500 MHz) δ 8.74 (s, 1H), 8.52 (s, 1H), 8.14 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08946237B2 |
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| 출처 데이터셋 | uspto-grants-2015_02 |
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| ORD ID | ord-d2d13dc2b371450b93e0b6e18f022f55 |
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| 출처 메모 | uspto-grants-2015_02 |
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