반응식
CC(=O)Nc1cc(N)ccc1N1CC[C@@H](NC(=O)OC(C)(C)C)C1.N#Cc1cnn2c(NC3CC3)cc(Cl)nc12>CC(C)c1cc(C(C)C)c(-c2ccccc2P(C(C)(C)C)C(C)(C)C)c(C(C)C)c1.CN1CCCC1=O.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C([O-])[O-].[Cs+].[Cs+].[Pd].[Pd]>CC(=O)Nc1cc(Nc2cc(NC3CC3)n3ncc(C#N)c3n2)ccc1N1CC[C@@H](N)C1참가 물질
반응물 2
생성물 1
시약·촉매·용매 4
반응 조건
- 온도
- 105 °C
실험 절차
5-chloro-7-(cyclopropylamino)pyrazolo[1,5-a]pyrimidine-3-carbonitrile (300 mg, 1.28 mmol), (R)-tert-butyl 1-(2-acetamido-4-aminophenyl)pyrrolidin-3-ylcarbamate (429 mg, 1.28 mmol), CESIUM CARBONATE (837 mg, 2.57 mmol) and di-tert- butyl(2',4',6'-triisopropylbiphenyl-2-yl)phosphine (54.5 mg, 0.13 mmol) were added into NMP (6 mL) in a 50mL round bottle. Pd2dba3 (58.8 mg, 0.06 mmol) was added to the solution. The solution was purged by nitrogen, then heated at 105°C overnight. Crude product was separarted between water and ethyl acetate. The organic layer was concentrated under reduced pressure. The crude product was purified on the ISCO(17g silica column, EA/hex 0-75%). Then the intermediate was put in 1N HCl in ether(5mL),. The solution was stirred at rt for2hrs. Crude product was purified on Gilson(0.1%TFA CH3CN/water 2-35%), 124.8mg final product was obtained as white solid
출처 및 근거
- ORD 기록
- ord-afce2c60bcdc4fe1bfc6b3962146067d
- 출처 데이터셋
- 750 AstraZeneca ELN dataset
- 원본 링크
- 출처 보기
연결된 노트
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