反応式
O[O:2][S:3]([O-:5])=O.[K+].[CH3:7][O:8][C:9]([C:11]1[C:16](S)=[CH:15][N:14]=[C:13](C)[N:12]=1)=[O:10].CO.[CH2:21]1COCC1>>[CH3:7][O:8][C:9]([C:11]1[CH:16]=[CH:15][N:14]=[C:13]([S:3]([CH3:21])(=[O:5])=[O:2])[N:12]=1)=[O:10]参加物
4
実験手順
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 g, 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.
後処理
- customThe resulting suspension is partitioned between methylene chloride and water
- additionwith the addition of NaOH and re
- extractionextracted with solvent
- customThe combined organic layers are dried
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-17e4af372e4346f2ac5c06e1cb231206
- 出典データセット
- uspto-grants-2004_05
- 特許番号
- US06730668B2
関連ノート
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