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MeOH tetrahydrofuran → Methyl 2-(methylsulfonyl)pyrimidine-4-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | MeOH tetrahydrofuran | HCID 21899815 | — |
| 反応物 | Potassium hydroxy sulfite | HCID 23707502 | — |
| 反応物 | 2-Methyl-sulfanyl-pyrimidine-4-carboxylic acid methyl ester | HCID 69222019 | — |
| 生成物 | Methyl 2-(methylsulfonyl)pyrimidine-4-carboxylate | HCID 19868790 | — |
反応手順
An aqueous solution (1 L) of Oxone® (211.7 g, 344 mmol) is added dropwise at 0° C. to a solution of 2-methyl-sulfanyl-pyrimidine-4-carboxylic acid methyl ester, 14, (19 9,86.1 mmol) in 1:1 methanol/THF (1 L). The reaction solution is allowed to warm to room temperature and stir for 1.5 hours. The resulting suspension is partitioned between methylene chloride and water. The aqueous phase is made alkaline with the addition of NaOH and re extracted with solvent. The combined organic layers are dried, filtered, and concentrated in vacuo to afford 18.4 g of the desired product as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087615B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-dead07a44f7a4bb99af3704ce3bf4d5d |
| 出典メモ | uspto-grants-2006_08 |