Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 2-Ethyl-4-pyrimidinamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylborane | HCID 7357 | — |
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | 2-Chloro-4-aminopyrimidine | HCID 345752 | — |
| 촉매 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Ethyl-4-pyrimidinamine | HCID 13925296 | 24.4% |
반응 단계
A 100-mL single-neck round-bottomed flask equipped with a magnetic stirrer and a reflux condenser was charged with 2-chloropyrimidin-4-amine (2.60 g, 20.0 mmol), triethylborane (20.0 mL, 1.0 M in THF, 20.0 mmol), Pd(dppf)Cl2 (816 mg, 1.0 mmol), K3PO4 (13.0 g, 40.0 mmol), water (2 mL), and tetrahydrofuran (50 mL). After three cycles of vacuum/argon flush, the mixture was heated at reflux for 14 h. It was then cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure and the resulting residue was purified by silica-gel column chromatography eluting with 40:1 dichloromethane/methanol to afford 229a as yellow solid (600 mg, 24%). MS-ESI: [M+H]+ 124.3
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09238655B2 |
| 출처 데이터셋 | uspto-grants-2016_01 |
| ORD ID | ord-bc12d6b4019e45538053503a395015a9 |
| 출처 메모 | uspto-grants-2016_01 |