Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethylamine → Methyl 3-amino-4-(2,6-dimethylphenylethynyl)-benzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethylamine | HCID 8021 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 2-Ethynyl-1,3-dimethylbenzene | HCID 13007669 | — |
| 반응물 | Methyl 3-amino-4-iodobenzoate | HCID 21628210 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 촉매 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl 3-amino-4-(2,6-dimethylphenylethynyl)-benzoate | HCID 66965741 | — |
반응 단계
A mixture of methyl 3-amino-4-iodobenzoate (920 mg, 3.32 mmol), 2,6-dimethylphenylacetylene (540 mg, 4.15 mmol),), bis-(triphenylphosphine) palladium (II) chloride (47 mg, 67 μmol), diethylamine (486 mg, 66 mmol), and copper (I) iodide (19 mg, 100 μmol) in DMF (10 mL) was heated at 120° C. in a microwave apparatus for 10 min. The mixture was poured into ethyl acetate and extracted six times with brine. The organic phase was dried, filtered, and the solvent was removed under reduced pressure to leave a residue that was chromatographed using a gradient of 0-30% heptane/ethyl acetate to afford methyl 3-amino-4-(2,6-dimethylphenylethynyl)-benzoate.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08222248B2 |
| 출처 데이터셋 | uspto-grants-2012_07 |
| ORD ID | ord-1f95b15787b8488a885bd3de7e50aa83 |
| 출처 메모 | uspto-grants-2012_07 |