Methyl iodide → 3,5-Dimethoxy-N-methylbenzenamine
反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:7]=[C:8]([O:10][CH3:11])[CH:9]=1)[NH2:6].IC.[C:14]([O-])(=O)C.[Na+]>C1COCC1>[CH3:11][O:10][C:8]1[CH:7]=[C:5]([NH:6][CH3:14])[CH:4]=[C:3]([O:2][CH3:1])[CH:9]=1参加物
5
実験手順
A solution of 3,5-dimethoxyaniline (13.8 g, 90 mmol), Iodomethane (12.7 g, 90 mmol), and sodium acetate (7.4 g, 90 mmol) in 100 ml of anhydrous THF was stirred under nitrogen atmosphere for 10 hr. Then, THF was removed by rotary evaporation. The crude product was partitioned between water and ethyl ether. The ethereal extraction was separated and washed with water, brine, and dried over Na2SO4. Filtration and removal of solvent provided 13.6 g of crude product. The crude product was chromatographed on silica gel (33% acetone-petroleum ether) to afford the expected product 4.5 g (27% yield).
後処理
- customThen, THF was removed by rotary evaporation
- customThe crude product was partitioned between water and ethyl ether
- extractionThe ethereal extraction
- customwas separated
- washwashed with water, brine
- dry with materialdried over Na2SO4
- filtrationFiltration and removal of solvent
- customprovided 13.6 g of crude product
- customThe crude product was chromatographed on silica gel (33% acetone-petroleum ether)
出典と根拠
- ORDレコード
- ord-0736f5026ca84458909cfdd1c9391405
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07183313B2
反応ノート
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