関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Amino-2-methyl-5-pyrimidinemethanamine | HCID 66762 | — |
| 反応物 | 4-Hydroxy-6-methyl-2-pyrone | HCID 54675757 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 54724214 | HCID 54724214 | 58.6% |
反応手順
A mixture of 4-hydroxy-6-methyl-2-pyrone (0.9 g, 0.007 mol) and 4-amino-5-aminomethyl-2-methylpyrimidine (1.0 g, 0.007 mol) in water (10.0 ml) was heated at 100° C. for 1 h under argon atmosphere. The reaction mixture was cooled, and filtered the yellow precipitate. It was washed successively with cold water, ethanol, and dried in vacuo to afford the title compound (1.01 g, 51%) as a pale yellow powder: 1H NMR (DMSO-d6/400 MHz) δ 7.62 (s, 1H), 7.04 (s, 1H), 5.83 (d, 1H, J=2.0 Hz), 5.58 (d, 1H, J=2.0 Hz), 4.92 (s, 2H), 2.24 (s, 3H), and 2.22 (s, 3H); ES-HRMS m/z 325.0304 (M+H C12H14N4O2Br requires 325.0295). Step 2 1-[(4-amino-2-methylpyrimidin-5-yl)methyl]-3-bromo-4-hydroxy-6-methylpyridin-2(1H)-one
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07067540B2 |
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| 出典データセット | uspto-grants-2006_06 |
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| ORD ID | ord-3dba739c2a4d4cffbeddd87551f97052 |
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| 出典メモ | uspto-grants-2006_06 |
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