참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | tert-Butyl carbamate | HCID 77922 | — |
| 반응물 | 2-Chloro-3-fluoro-5-methylpyridine | HCID 13541365 | — |
| 시약 | Sodium Hydroxide | HCID 14798 | — |
| 촉매 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 촉매 | Palladium (II) acetate | HCID 4144353 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | tert-butyl N-(3-fluoro-5-methyl-2-pyridinyl)carbamate | HCID 90064798 | 25.74% |
반응 단계
diacetoxypalladium (15.42 mg, 0.07 mmol) and(9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (39.8 mg, 0.07 mmol) were added to a degassed mixture of 2-chloro-3-fluoro-5-methylpyridine (100 mg, 0.69 mmol), tert-butyl carbamate (105 mg, 0.89 mmol) and 2-chloro-3-fluoro-5-methylpyridine (100 mg, 0.69 mmol) in dioxane (10 mL) at 21°C. The resulting mixture was stirred at 100 °C for 2 hours.Cooled. Adsorbed onto silica. The crude product was purified by flash silica chromatography, elution gradient 10 to 30% DCM in heptane. Pure fractions were evaporated to dryness to afford tert-butyl 3-fluoro-5-methylpyridin-2-ylcarbamate (40.0 mg, 25.7 %) as a cream solid. not pure enough to register ..
출처 및 근거
| 출처 데이터셋 | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-fde5e0f95519439ca9660af435fc14a6 |
|---|
| 출처 메모 | 750 AstraZeneca ELN dataset |
|---|