Diethyl Ether → P-Toluic Acid
反応式
Br([O-])(=O)=O.[Na+].[CH3:6][C:7]1[CH:14]=[CH:13][C:10]([CH2:11][OH:12])=[CH:9][CH:8]=1.CC[O:17]CC>C(#N)C.O>[CH3:6][C:7]1[CH:14]=[CH:13][C:10]([C:11]([OH:17])=[O:12])=[CH:9][CH:8]=1参加物
5
反応条件
- 温度
- 80 °C
実験手順
A mixture of Ceiv catalyst from Example 47 (0.08 g), sodium bromate (0.3 g) and 4-methylbenzyl alcohol (0.24 g, 2 mmol) in acetonitrile:water (1:1, 10 ml) was stirred at 80° C. for 40 h under an atmosphere of nitrogen. On cooling ether (70 ml) was added and the catalyst was filtered off. The organic layer was separated and the aqueous phase was extracted with ether (2×50 ml). The combined organic extracts were washed with water (25 ml), dried with anhydrous magnesium sulphate and concentrated to give 4-methylbenzoic acid as a white solid (0.26 g, 96%). M.p. 178° C., lit. 180-182° C.
後処理
- additionwas added
- filtrationthe catalyst was filtered off
- customThe organic layer was separated
- extractionthe aqueous phase was extracted with ether (2×50 ml)
- washThe combined organic extracts were washed with water (25 ml)
- dry with materialdried with anhydrous magnesium sulphate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-3a9fbafd96bf492091f8f6f9a3668ff1
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07728159B2
反応ノート
読み込み中…