참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Binap, (A+-)- | HCID 634876 | — |
| 반응물 | 3-Bromo-4-phenylpyridine | HCID 2762928 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 반응물 | 5-Amino-2-butyl-2,3-dihydro-1H-isoindol-1-one | HCID 67432065 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-Butyl-5-(4-phenylpyridin-3-ylamino)isoindolin-1-one | HCID 53477129 | 46% |
반응 단계
3-Bromo-4-phenylpyridine (125 mg, 0.534 mmol) was added to a suspension of 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (BINAP) (33 mg, 0.053 mmol) and tris(dibenzylideneacetone)dipalladium(0) (Pd2(dba)3) (49 mg, 0.053 mmol) in toluene (5 mL). 5-Amino-2-butylisoindolin-1-one (120 mg, 0.587 mmol) and sodium tert-butoxide (128 mg, 1.335 mmol) were added and the mixture was stirred and heated in the microwave (120° C., 300 W, 75 min). Water and ethyl acetate were added, the organic layer was separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with water and dried over MgSO4. Purification by flash chromatography (dichloromethane/methanol, gradient 1-5% methanol) provided 2-butyl-5-(4-phenylpyridin-3-ylamino)isoindolin-1-one (56 mg, 46%). ESI-MS [M+H]+=358.2.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08314120B2 |
|---|
| 출처 데이터셋 | uspto-grants-2012_11 |
|---|
| ORD ID | ord-91b69fd51ec14050860577b9e1cd9ae3 |
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| 출처 메모 | uspto-grants-2012_11 |
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