化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 5,6-Dimethylthieno[2,3-d]pyrimidine-2,4-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Amino-4,5-dimethyl-thiophene-3-carbonitrile | HCID 290236 | — |
| 反応物 | HCID 178418324 | HCID 178418324 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5,6-Dimethylthieno[2,3-d]pyrimidine-2,4-diamine | HCID 12659533 | 5.2% |
反応手順
A mixture of 2-amino-4,5-dimethylthiophene-3-carbonitrile (500 mg, 3.29 mmol), cyanoguanidine (276.6 mg, 3.29 mmol) and HCl (2 N, 1.5 mL) in water (10 mL) was refluxed under nitrogen for 2 h. The reaction mixture was cooled to room temperature, and basified with diluted NaOH aqueous solution to PH 7˜8. After evaporation of water, the residue was purified by preparative HPLC eluting with acetonitrile and water to give the title compound (33 mg, 5%). 1H NMR (400 MHz, DMSO-d6) δ2.22 (s, 3H), 2.27 (s, 3H), 5.85 (bs, 2H), 6.29 (bs, 2H). MS 195 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541421B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-2106847e217d4fd886bd312d278c22c4 |
| 出典メモ | uspto-grants-2013_09 |