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Formamide → thieno(2,3-d)pyrimidin-4(3H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formamide | HCID 713 | — |
| 反応物 | Methyl 2-amino-3-thenoate | HCID 78381 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | thieno(2,3-d)pyrimidin-4(3H)-one | HCID 2808547 | 40% |
反応手順
A solution of methyl 2-aminothiophene-3-carboxylate (602.1 mg, 3.83 mmol) in formamide (5 mL) is heated at 200° C. for 12 h. The resulting tar is dissolved in CH2Cl2 (10 mL) then placed on a silica plug and eluted with 10% MeOH in CH2Cl2. The filtrate is stripped under reduce pressure and the resulting solid is washed with EtOH to yield 3H-thieno[2,3-d]pyrimid-4-one (231.4 mg, 40%) as an orange solid. 1H NMR (DMSO) δ 12.50 (1H, brs), 8.13 (1H, s), 7.60 (1H, d, J=5.8 Hz), 7.41 (1H, d, J=6.0 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06713484B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-ec81770f988643769db832e9958cef58 |
| 出典メモ | uspto-grants-2004_03 |