참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methylhydrazine | HCID 6061 | — |
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Methyl pyrimidine-4-carboxylate | HCID 254248 | — |
| 반응물 | 4-Bromo-2-methylbenzaldehyde | HCID 13555150 | — |
| 반응물 | HCID 86724095 | HCID 86724095 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 86724094 | HCID 86724094 | 51% |
반응 단계
To the suspension of 1-methyl-3-(pyrimidin-4-yl)-1H-pyrazol-5-amine (0.42 g, 2.4 mmol, prepared using A with methylpyrimidine-4-carboxylate (Ark Pharm) with NaH followed by B with methyl hydrazine) and 4-bromo-2-methylbenzaldehyde (0.48 g, 2.40 mmol, Ark Pharm) in acetonitrile (15 mL) was added p-TSA (0.09 g, 0.5 mmol) and heated to about 50° C. for about 5 h. The reaction mixture was cooled to ambient temperature and continued to stir for about 16 h. The precipitate was collected by filtration and dried under reduced pressure to afford 4-(4-bromo-2-methylbenzylidene)-1-methyl-3-(pyrimidin-4-yl)-1H-pyrazol-5(4H)-imine (0.43 g, 51%) as a light brown solid. LC-MS MS (Table 1, Method g) Rt=2.48 min, m/z 356, 358 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09150592B2 |
|---|
| 출처 데이터셋 | uspto-grants-2015_10 |
|---|
| ORD ID | ord-cc7b99e24e194ba2bab0c8920f565776 |
|---|
| 출처 메모 | uspto-grants-2015_10 |
|---|
