関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 1,1,1-Trimethoxybutane | HCID 123512 | — |
| 反応物 | 2-Chloro-4,5-diamino-6-methylpyrimidine | HCID 275295 | — |
| 溶媒 | 2-Methoxyethanol | HCID 8019 | — |
| 生成物 | 2-Chloro-6-methyl-8-propylpurine | HCID 19012212 | 47.1% |
反応手順
A mixture of 2-Chloro-4,5-diamino-6-methylpyrimidine (0.80 g, 5.04 mmol), trimethylorthobutyrate (1.2 ml, 7.6 mmol) and p-TsOH (0.08 g) in 2-methoxyethanol (24 ml) was heated in an oil bath at 140° C. for 24 hours. The product was isolated as described in Step 2 of Example 12 and purified by flash chromatography using EtOAc-hexane (1:1) to give the crystalline titled compound (0.5 g, 47%). NMR (CDCl3): δ1.03 (t, J=8 Hz,3H), 1.9 (q,2H), 2.82 (s, 3H), 3.0 (t, J=8 Hz, 2H). FAB-MS: m/e 211 and 213 (M+H). Analysis calculated for C9H11N4Cl: C, 51.31; H, 5.26; N, 26.60. Found: C, 51.43; H, 5.50, N, 26.81.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05102880 |
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| 出典データセット | uspto-grants-1992_04 |
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| ORD ID | ord-8759ea6a42a84a318ec38a8945ae7b4d |
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| 出典メモ | uspto-grants-1992_04 |
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