참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 6-Chloro-3-methylpyrimidin-4(3H)-one | HCID 4366471 | — |
| 반응물 | 2,6-Dimethyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline | HCID 56737724 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 6-(4-Amino-3,5-dimethylphenyl)-3-methylpyrimidin-4(3H)-one | HCID 86697249 | — |
반응 단계
In a microwave vial 2,6-dimethyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (5.6 g) and 6-chloro-3-methylpyrimidin-4(3H)-one (3 g) are suspended in N,N-dimethylformamide (30 mL) and Na2CO3 (26 mL of a 2M aqueous solution). The mixture is purged for 5 minutes with argon. [1,1′-Bis(diphenylphosphino)-ferrocene]-dichloropalladium dichloromethane complex (508 mg) is added, the vial is sealed and the mixture is stirred at 65° C. for 12 hours. After cooling to room temperature the mixture is Partitioned between water and ethyl acetate. The aqueous phase is extracted twice with ethyl acetate and the combined organic phases are washed with brine and dried (MgSO4). The solvents are evaporated to give the title compound. Yield: 2.6 g; LC (method 11): tR=0.71 min; Mass spectrum (ESI+): m/z=230 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08642585B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-c31715c430bd41598881d2f21c3a7fac |
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| 출처 메모 | uspto-grants-2014_02 |
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