Methylamine → [2-(2-Methoxyphenoxy)ethyl](methyl)amine
反応式
Br[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[O:11][CH3:12].[CH3:13][NH2:14]>C(O)C>[CH3:12][O:11][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=1[O:4][CH2:3][CH2:2][NH:14][CH3:13]参加物
4
実験手順
A solution of 1-(2-bromoethoxy)-2-methoxybenzene (7d) (7.7 g, 33 mmol) in a 33% solution of methylamine in ethanol was heated at 80° C. in a sealed tube for 16 h. After cooling to room temperature, the solvents were evaporated in vacuo. A 2N aqueous solution of sodium hydroxide was added to the remaining oil and the resulting slurry was extracted with ethyl acetate (2×250 mL). The collected organic phases were dried (Na2SO4) and the solvents evaporated in vacuo giving 5.9 g (98%) of the title compound as an oil: 1H NMR (CDCl3) δ 1.85 (broad s, 1H), 2.50 (s, 3H), 3.00 (t, 2H), 3.85 (s, 3H), 4.10 (t, 2H), 6.85-6.95 (m, 4H).
後処理
- customthe solvents were evaporated in vacuo
- additionA 2N aqueous solution of sodium hydroxide was added to the remaining oil
- extractionthe resulting slurry was extracted with ethyl acetate (2×250 mL)
- dry with materialThe collected organic phases were dried (Na2SO4)
- customthe solvents evaporated in vacuo
出典と根拠
- ORDレコード
- ord-4c46427fac9a43dbbac67362b16ecd82
- 出典データセット
- uspto-grants-2002_12
- 特許番号
- US06492374B2
反応ノート
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