Methyl iodide → HCID 58396979、化合物
反応式
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]([CH2:11][CH3:12])([CH3:10])[CH3:9])[CH:5]=[CH:4][C:3]=1[OH:13].[C:14](=O)([O-])[O-].[K+].[K+].CI>CN(C=O)C.CCOC(C)=O>[CH3:14][NH:1][C:2]1[CH:7]=[C:6]([C:8]([CH2:11][CH3:12])([CH3:9])[CH3:10])[CH:5]=[CH:4][C:3]=1[OH:13]参加物
6
実験手順
2-Amino-4-tert-pentylphenol (5.00 g, 27.8 mmol) and potassium carbonate (3.88 g, 28.1 mmol) were mixed at RT for 2.5 hours in DMF (15 mL). Methyl iodide (1.20 mL, 19.3 mmol) was added and the mixture was stirred overnight at RT. Diluted the mixture with EtOAc and extracted with aqueous sodium bicarbonate and water. Dried the organic layers over sodium sulfate, filtered, concentrated and purified by silica gel chromatography (10-15% MTBE/hexanes). Concentrated the product fractions to yield the title compound.
後処理
- extractionextracted with aqueous sodium bicarbonate and water
- dry with materialDried the organic layers over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- custompurified by silica gel chromatography (10-15% MTBE/hexanes)
- concentrationConcentrated the product fractions
出典と根拠
- ORDレコード
- ord-298b0fbe0a004ee59bbbeaef43e84fc4
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08476434B2
反応ノート
読み込み中…