참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Indole | HCID 798 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | Methylboronic Acid | HCID 139377 | — |
| 촉매 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4,6-dimethyl-1H-indole-3-carboxylic acid | HCID 82404736 | 40.9% |
반응 단계
A mixture of indole 5 (690 mg, 3.28 mmol), methylboronic acid (495 mg, 3.94 mmol, 1.2 eq.), Pd(dppf)Cl2 (180 mg, 0.656 mmol, 0.2 eq.) and Cs2CO3 (3.20 g, 9.84 mmol, 3.0 eq.) in dioxane (21 mL) and water (3 mL) was stirred at 110° C. overnight under N2. The mixture was diluted with water and extracted with EtOAc. The combined extracts were washed with brine, dried over Na2SO4 and concentrated. The residue was purified by silica gel chromatography (petroleum ether/EtOAc=5/1) to give the desired product (170 mg, 1.17 mmol, 40.9%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09434724B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_09 |
|---|
| ORD ID | ord-863bbacc59ae4f1498b0036fe5995fc5 |
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| 출처 메모 | uspto-grants-2016_09 |
|---|
