참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate Monohydrate | HCID 2735133 | — |
| 반응물 | 2-Fluoropyridine-3-boronic acid | HCID 2783270 | — |
| 반응물 | (4-(3-chloropyrazin-2-yloxy)phenyl)(1H-benzo[d]imidazol-2-yl)methanone | HCID 46207940 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | HCID 59351416 | HCID 59351416 | — |
반응 단계
To a microwave safe 30 ml tubes were charged with (1H-benzo[d]imidazol-2-yl)(4-(3-chloropyrazin-2-yloxy)phenyl)methanone (0.500 g, 1.43 mmol), 2-fluoropyridin-3-ylboronic acid (0.241 g, 1.71 mmol), tetrakis(triphenylphosphine)palladium(0) (0.165 g, 0.143 mmol) and a 2M solution of sodium carbonate monohydrate (2.14 mL, 4.28 mmol) in 1,4-dioxane. The flasks were sealed and heated to 150° C. for 45 min in a microwave. The reaction mixture was diluted with DCM (75 mL), washed with water and brine. It was dried over magnesium sulfate, concentrated and dried in vacuo. It was suspended in DCM/MeOH and stirred. The insoluble material was collected by filtration, recrystallized overnight from boiling MeOH and hexane, then dried in a vacuum oven to give (1H-benzo[d]imidazol-2-yl)(4-(3-(2-fluoropyridin-3-yl)pyrazin-2-yloxy)phenyl)methanone as yellow solid. LC/MS: MS (ESI, pos. ion) m/z: 412.1 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08053438B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_11 |
|---|
| ORD ID | ord-d8a465e9d6a64a44a82b25f6ae88332a |
|---|
| 출처 메모 | uspto-grants-2011_11 |
|---|