関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (4-Chloro-2-(methylthio)pyrimidin-5-yl)methanol | HCID 59419388 | — |
| 触媒 | HCID 178418406 | HCID 178418406 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 4-Chloro-2-(methylsulfanyl)pyrimidine-5-carbaldehyde | HCID 59419386 | 72% |
反応手順
(4-Chloro-2-(methylthio)pyrimidin-5-yl)methanol (105 mmol) was dissolved in CHCl3 (500 mL) to give a yellow suspension. Manganese(IV) oxide (546 mmol) was added in 0.5 g portions over 15 min. The mixture was stirred at room temperature for 6 h. Further Manganese(IV) oxide (210 mmol) was added. The mixture was stirred at room temperature for 18 h. Again, manganese(IV) oxide (210 mmol) was added. The mixture was stirred at room temperature for 20 h, then at 40° C. for 4 h, and then overnight at room temperature. The mixture was then stirred at 40° C. for 6 h, allowed to cool to room temperature, filtered though Celite, washed with 400 mL CHCl3 and concentrated under reduced pressure to give 4-chloro-2-(methylthio)pyrimidine-5-carbaldehyde as a solid (72%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08232283B2 |
|---|
| 出典データセット | uspto-grants-2012_07 |
|---|
| ORD ID | ord-effb7cb4d546489cb7b260a983f66477 |
|---|
| 出典メモ | uspto-grants-2012_07 |
|---|