Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 4-bromo-1-(tris(4-methoxyphenyl)methyl)-1H-pyrazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Bromopyrazole | HCID 16375 | — |
| 반응물 | 4,4',4''-Trimethoxytrityl chloride | HCID 630505 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-bromo-1-(tris(4-methoxyphenyl)methyl)-1H-pyrazole | HCID 58432066 | 52% |
반응 단계
To a suspension of 4-bromopyrazole (1.5 g, 10.2 mmol) and 4,4′,4″-trimethoxytrityl chloride (4.5 g, 12.2 mmol) in anhydrous DMF (20 mL) under argon was added triethylamine (3 mL, 21.5 mmol) and the mixture was cooled over an ice bath. After stirring for 10 min, the ice bath was removed and the reaction stirred for 2.5 hrs. The mixture was diluted with H2O and extracted with EtOAc. The combined organics were washed with H2O three times then saturated aqueous NaHCO3 and brine. The solution was dried over Na2SO4 and concentrated in vacuo. The crude oil was recrystallized from isopropanol to give 4-bromo-1-(tris(4-methoxyphenyl)methyl)-1H-pyrazole as off-white crystals (two batches; 2.55 g, 52% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09434707B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-e22b13b5bfdd44da9a4dce6762ee6bc5 |
| 출처 메모 | uspto-grants-2016_09 |