반응식
CCNc1ccccc1.COc1nc(I)ncc1Br>CC(=O)O.CC(=O)O.CC1(C)c2cccc(P(c3ccccc3)c3ccccc3)c2Oc2c(P(c3ccccc3)c3ccccc3)cccc21.CCC(C)(C)[O-].Cc1ccccc1.[Na+].[Pd]>CCN(c1ccccc1)c1ncc(Br)c(OC)n1참가 물질
반응물 2
생성물 1
시약·촉매·용매 4
반응 조건
- 온도
- 100 °C
실험 절차
5-bromo-2-iodo-4-methoxypyrimidine (0.086 g, 0.27 mmol), diacetoxypalladium (2.78 mg, 0.01 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) - XantPhos (7.16 mg, 0.01 mmol) and sodium 2-methylbutan-2-olate (0.055 g, 0.50 mmol) and di((3S,5S,7S)-adamantan-1-yl)(butyl)phosphine (8.88 mg, 0.02 mmol) were added to a micro vial. Then N-ethylaniline (0.031 mL, 0.25 mmol) in toluene (1.5 mL) was added to the reaction mixture. The vial was sealed and evacuated and flushed with nitrogen and then stirred at 100°C o/n. LC/MS showed product formation. The reaction mixture was cooled to rt and then filtered over celite. The crude product was diluted with 25 ml of DCM and then washed with sat. NaHCO3 followed by brine. The organic phase was dried over a phase separator and then concentrated to dryness. **No LC/MS data due to database failure over three months and was only saved locally on LC/MS computer and pdf-files seems to be deleted on machine. Not used in further reactions.**
출처 및 근거
- ORD 기록
- ord-3df00475fe9d41898bd3503e3b2ed03d
- 출처 데이터셋
- 750 AstraZeneca ELN dataset
- 원본 링크
- 출처 보기
연결된 노트
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