참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 5-Bromo-2-chloro-N-(tetrahydro-2H-pyran-4-yl)pyrimidin-4-amine | HCID 59550890 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | 5-Bromo-N4-(tetrahydro-pyran-4-yl)-pyrimidine-2,4-diamine | HCID 58299673 | 77% |
반응 단계
To a suspension of compound 32 (6.60 g, 23 mmol) in isopropyl alcohol (40 ml) was added ammonia (aq. 28%, 80 ml). This reaction mixture was heated to 130° C. for 14 hours in a pressure vessel. The reaction mixture was cooled down to room temperature and to this mixture was added ethyl acetate. The reaction mixture was washed with water and brine. The ethyl acetate layer was dried with sodium sulfate and concentrated to give compound 33 (4.75 g, 77%). 1H NMR (500 MHz, CD3OD) δ ppm 7.79 (1 H, s), 4.24 (1 H, m), 3.99-4.02 (2 H, dd, J=11.0, 2.2 Hz), 3.52 (2 H, td, J=11.9, 2.0 Hz), 1.92-1.96 (2 H, m), 1.69 (2 H, m); LCMS-ESI (POS), M/Z, M+1: Found 273, Calculated 273.0
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08841312B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-6229f9a396354562be7e42eb4230bbe6 |
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| 출처 메모 | uspto-grants-2014_09 |
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