참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-Methylbut-1-yne | HCID 69019 | — |
| 반응물 | Ethyl 3-amino-4-iodobenzoate | HCID 59762281 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | Ethyl3-Amino-4-(3-methylbut-1-ynyl)benzoate | HCID 59762350 | — |
반응 단계
To a solution of ethyl3-amino-4-iodobenzoate (Compound 31, 6.87 g, 23.1 mmol) in triethylamine (50 ml) at 25° C. under argon then added CuI (22 mg, 1.16 mmol), Pd(PPh3)2Cl2 (82 mg, 1.16 mmol), and 3-methyl-1-butyne ( 3.18 g, 46.2 mmol). The reaction was stirred for 20 h at 25° C., filtered off brown solid, and then rinsed solid with EtOAc, organic layer was concentrated in vacuo. The residue was purified by chromatography on silica gel (0→25% EtOAc-hexanes) to yield the title compound as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08524917B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_09 |
|---|
| ORD ID | ord-8cfdaf0063bc4f8ba461f5f905e1d324 |
|---|
| 출처 메모 | uspto-grants-2013_09 |
|---|