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Chloroform → 4-Chloro-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 2-Amino-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4(3h)-one | HCID 290197 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | 4-Chloro-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-2-amine | HCID 12910200 | 44% |
反応手順
To a 50 mL flask was added 10 (221 mg, 1 mmol) and 10 mL POCl3. The resulting mixture was refluxed for 2 h, and the solvent was removed under reduced pressure to afford a dark residue. To this was added 30 mL of CHCl3 and 300 mg of silica gel. The solvent was evaporated to afford a plug. Column chromatography of the plug with hexane: acetyl acetate=20:1 as eluent afford 105 mg (44%) of 11 as a yellow solid:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09056869B2 |
| 出典データセット | uspto-grants-2015_06 |
| ORD ID | ord-4357a1e6bed444b79c90c45b72e89348 |
| 出典メモ | uspto-grants-2015_06 |