関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Amino-2-(methylsulfanyl)pyrimidine-5-carbaldehyde | HCID 295769 | — |
| 反応物 | (3-Amino-2,6-dichloro-phenyl)-acetonitrile | HCID 23185255 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 59860298 | HCID 59860298 | 80% |
反応手順
A mixture of 4-amino-2-methylsulfanyl-pyrimidine-5-carbaldehyde (2.0 g, 11.82 mmol), (3-amino-2,6-dichloro-phenyl)-acetonitrile (2.85 g, 14.18 mmol) and K2CO3 (4.9 g, 35.49 mmol) in DMF (20 mL) is heated to 110° C. for 30 hours. The solution is cooled to room temperature and the solid is removed by filter paper and concentrated to give crude product. Flash silica gel column purification, eluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/7%), gives the title intermediate as a solid (3.31 g, 80.0%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07449582B2 |
|---|
| 出典データセット | uspto-grants-2008_11 |
|---|
| ORD ID | ord-e4f4a8f10e67450f8d1fa16affa1cd13 |
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| 出典メモ | uspto-grants-2008_11 |
|---|
