Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 6-chloro-N-(4-hydroxy-2-methylphenyl)pyrimidine-4-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Amino-m-cresol | HCID 17819 | — |
| 반응물 | 6-Chloropyrimidine-4-carbonyl chloride | HCID 18422098 | — |
| 반응물 | 6-chloro-N-(4-hydroxyphenyl)pyrimidine-4-carboxamide | HCID 59446876 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 6-chloro-N-(4-hydroxy-2-methylphenyl)pyrimidine-4-carboxamide | HCID 59447105 | — |
반응 단계
A cooled (0° C.) solution of 4-amino-m-cresol (Fluka, 4.17 g, 33.9 mmol) and triethylamine (23.6 mL, 0.170 mol) in dry dichloromethane (100 mL) was treated with 6-chloropyrimidine-4-carbonyl chloride, obtained as described above for Intermediate 7, step 1 (6.0 g, 34 mmol) and the resulting mixture was stirred at room temperature for 12 hours. The reaction mixture was concentrated in vacuo, diluted with water and extracted with EtOAc. The combined organic layers were dried on magnesium sulfate and evaporated in vacuo. The crude product was purified by column chromatography (silica) using as eluent petroleum ether/EtOAc to afford the title compound as yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08399448B2 |
| 출처 데이터셋 | uspto-grants-2013_03 |
| ORD ID | ord-293e601e98894baca4aea202277ee4ff |
| 출처 메모 | uspto-grants-2013_03 |