関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 5-Bromo-2-chloro-N-(tetrahydro-2H-pyran-4-yl)pyrimidin-4-amine | HCID 59550890 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 5-Bromo-N4-(tetrahydro-pyran-4-yl)-pyrimidine-2,4-diamine | HCID 58299673 | 77% |
反応手順
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
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08841312B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-6229f9a396354562be7e42eb4230bbe6 |
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| 出典メモ | uspto-grants-2014_09 |
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