Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Iodide → Methyl 4-((di-tert-butoxyphosphoryloxy)methyl)benzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Methyl 4-(bromomethyl)benzoate | HCID 256687 | — |
| 반응물 | Potassium di-tert-butyl phosphate | HCID 23674467 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl 4-((di-tert-butoxyphosphoryloxy)methyl)benzoate | HCID 90087888 | — |
반응 단계
Methyl 4-(bromomethyl)benzoate (1200 mg, 5.24 mmol), potassium di-tert-butyl phosphate (1431 mg, 5.76 mmol) and sodium iodide (785 mg, 5.24 mmol) were combined in DMF (3.00 mL) under nitrogen. The reaction mixture was stirred at room temperature for 24 h. The reaction mixture was diluted with ether, washed with 10% LiCl solution and brine, then dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by silica gel chromatography (hexane/EtOAc) to provide Preparation 55A (571 mg, 1.593 mmol, 30%): 1H NMR (400 MHz, CDCl3) δ 8.03 (d, J=8.4 Hz, 2H), 7.53-7.37 (m, 2H), 5.05 (d, J=7.5 Hz, 2H), 3.92 (s, 3H), 1.48 (d, J=0.4 Hz, 18H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09242941B2 |
| 출처 데이터셋 | uspto-grants-2016_01 |
| ORD ID | ord-ddb14697f5774d0e8ba27545822bb64b |
| 출처 메모 | uspto-grants-2016_01 |