반응식
C1COCCN1.COCCOc1cc(I)cc([N+](=O)[O-])c1>CC(=O)O.CC(=O)O.Cc1ccccc1.O=C([O-])[O-].[Cs+].[Cs+].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>COCCOc1cc(N2CCOCC2)cc([N+](=O)[O-])c1참가 물질
반응 조건
- 온도
- 110 °C
실험 절차
diacetoxypalladium (0.136 g, 0.60 mmol) was added to a stirred mixture of 1-iodo-3-(2-methoxyethoxy)-5-nitrobenzene (3.9 g, 12.07 mmol), morpholine (1.373 mL, 15.69 mmol) and 2,2'-bis(diphenylphosphino)-1,1'-binaphthyl (0.225 g, 0.36 mmol) and cesium carbonate (11.80 g, 36.21 mmol) dissolved in toluene (100 mL) over a period of 5 minutes, degased and under argon. The resulting mixture was heated at 110 °C for 4 hours.The toluene was evaporated , water ( 50ml) was added and the mixture was extracted with ethyle acetate, dried over MgSO4, filtered and asorbed on silica gel.The crude product was purified by flash chromatography on silica gel eluting with 1 to 4% methanol in dichloromethane. The solvent was evaporated to dryness to afford 4-(3-(2-methoxyethoxy)-5-nitrophenyl)morpholine (0.550 g, 16.14 %) as a orange solid. ( starting material unreacted : 2 .5g)
출처 및 근거
- ORD 기록
- ord-5a683960052443b49da1956ac277ce2a
- 출처 데이터셋
- 750 AstraZeneca ELN dataset
- 원본 링크
- 출처 보기
연결된 노트
불러오는 중…