Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → Methyl 3-((2-iodophenethyl)amino)-2-methyl-3-oxopropanoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Propylphosphonic anhydride | HCID 111923 | — |
| 반응물 | 3-Methoxy-2-methyl-3-oxopropanoic acid | HCID 300693 | — |
| 반응물 | 2-(2-Iodophenyl)ethanamine | HCID 10514616 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Methyl 3-((2-iodophenethyl)amino)-2-methyl-3-oxopropanoate | HCID 86711343 | 78.5% |
반응 단계
A solution of T3P in AcOEt (50%, 26.2 mL, 44.0 mmol) was added dropwise at 0° C. under N2 to a clear solution of 2-(2-iodophenyl)ethanamine (9.45 g, 38.2 mmol), 3-methoxy-2-methyl-3-oxopropanoic acid (5.05 g, 38.2 mmol) and Et3N (10.7 mL, 76.0 mmol) in AcOEt (350 mL). The mixture was stirred at RT for 6 days. A 2N aqueous solution of NaOH (50 mL) was then added to the reaction and the mixture was extracted with AcOEt. The combined org. layers were then dried over Na2SO4, filtered and concentrated in vacuo. The yellow oil obtained was purified by flash chromatography (SiO2, cHEx/AcOEt 100:0 to 50:50) to afford the title compound (10.83 g) as a clear oil. UPLC-MS: MS 362.2 (M+H+); UPLC rt 0.95 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09284331B2 |
| 출처 데이터셋 | uspto-grants-2016_03 |
| ORD ID | ord-f8688558e29c4735b0c40bd716b90d10 |
| 출처 메모 | uspto-grants-2016_03 |