참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Morpholine | HCID 8083 | — |
| 반응물 | 1-Iodo-3-(2-methoxyethoxy)-5-nitro-benzene | HCID 59817811 | — |
| 시약 | Cesium carbonate | HCID 10796 | — |
| 촉매 | Binap, (A+-)- | HCID 634876 | — |
| 촉매 | Palladium (II) acetate | HCID 4144353 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 4-[3-(2-Methoxyethoxy)-5-nitrophenyl]morpholine | HCID 59817838 | 16.14% |
반응 단계
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
| 출처 데이터셋 | 750 AstraZeneca ELN dataset |
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| ORD ID | ord-5a683960052443b49da1956ac277ce2a |
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| 출처 메모 | 750 AstraZeneca ELN dataset |
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