참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 7-Chloropyrazolo[1,5-a]pyrimidin-5-amine | HCID 44251306 | — |
| 반응물 | 7-Chloro-2-methylpyrazolo[1,5-a]pyrimidin-5-amine | HCID 44251307 | — |
| 반응물 | 7-Chloro-2-ethylpyrazolo[1,5-a]pyrimidin-5-amine | HCID 44251308 | — |
| 반응물 | HCID 44251312 | HCID 44251312 | — |
| 반응물 | Terephthalic acid monomethylester chloride | HCID 53442854 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | Methyl 4-(7-chloropyrazolo[1,5-a]pyrimidin-5-ylcarbamoyl)benzoate | HCID 86652259 | 92% |
| 생성물 | Methyl 4-(7-chloro-2-methylpyrazolo[1,5-a]pyrimidin-5-ylcarbamoyl)benzoate | HCID 86652260 | 72% |
| 생성물 | Methyl 4-(7-chloro-2-ethylpyrazolo[1,5-a]pyrimidin-5-ylcarbamoyl)benzoate | HCID 86652261 | 84% |
| 생성물 | HCID 86652262 | HCID 86652262 | 98% |
반응 단계
7-Chloropyrazolo[1,5-a]pyrimidin-5-amine (1E, 1.0 equivalent), 7-chloro-2-methylpyrazolo[1,5-a]pyrimidin-5-amine (1J, 1.0 equivalent), 7-chloro-2-ethylpyrazolo[1,5-a]pyrimidin-5-amine (1O, 1.0 equivalent), or 7-chloro-2-cyclopropylpyrazolo[1,5-a]pyrimidin-5-amine (1S, 1.0 equivalent) was suspended in pyridine (0.3 M). At 0° C. was added terephthalic acid monomethylester chloride (2B, 1.3 equivalents), and the mixture was stirred vigorously at 0° C. for 4-18 h. The reaction was quenched with saturated NaHCO3 and stirred for another 0.5 h; pyridine was removed in vacuo and the residue was suspended in water. The precipitate was collected on a fritted glass funnel and was washed twice with water. After drying under a stream of N2 for 15 h, the crude product methyl 4-(7-chloropyrazolo[1,5-a]pyrimidin-5-ylcarbamoyl)benzoate 2C (92%), methyl 4-(7-chloro-2-methylpyrazolo[1,5-a]pyrimidin-5-ylcarbamoyl)benzoate 2E (72%), methyl 4-(7-chloro-2-ethylpyrazolo[1,5-a]pyrimidin-5-ylcarbamoyl)benzoate 2G (84%) or methyl 4-(7-chloro-2-cyclopropylpyrazolo[1,5-a]pyrimidin-5-ylcarbamoyl)benzoate 2I (98%) was obtained as an orange solid and was used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08921358B2 |
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| 출처 데이터셋 | uspto-grants-2014_12 |
|---|
| ORD ID | ord-53a357503d2a448d8761ad4e1d76117f |
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| 출처 메모 | uspto-grants-2014_12 |
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