反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH3:10])[CH:4]=1.CN(C)CCN(C)C.C([N-]CC)C.[K+].[C:25](=[O:27])=[O:26]>C(N(CC)CC)C.O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH3:10])[C:4]=1[C:25]([OH:27])=[O:26]参加物
実験手順
A solution of 1,3-dimethoxybenzene (12.06 g.) and tetramethylethylenediamine (15 ml.) in triethylamine (20 ml.) was added to the potassium diethylamide reaction mixture and stirred for two hours. The entire mixture, a gray suspension, was poured into a 1-liter beaker containing crushed dry ice (456 g.) with the aid of 35 ml of added triethylamine and was allowed to warm to room temperature. The contents of the beaker were transferred into a 1-liter flask with the aid of some water. All volatile components were removed by a rotary evaporator. The solid remaining in the flask was partitioned between diethyl ether (30 ml.) and water, which was extracted with diethyl ether (four times, 30 ml.). The aqueous layer was acidified with concentrated hydrochloric acid to a pH of 1. The resultant precipitate was collected by filtration, water-washed and air dried to give 10.99 g. (69% yield) of 2,6-dimethoxybenzoic acid.
後処理
- additionThe entire mixture, a gray suspension, was poured into a 1-liter beaker
- additioncontaining
- customAll volatile components were removed by a rotary evaporator
- customwas partitioned between diethyl ether (30 ml.) and water, which
- extractionwas extracted with diethyl ether (four times, 30 ml.)
- filtrationThe resultant precipitate was collected by filtration, water-
- washwashed
- customair dried
- customto give 10.99 g
出典と根拠
- ORDレコード
- ord-099de03743944935877b63130f78306e
- 出典データセット
- uspto-grants-1989_07
- 特許番号
- US04845276
関連ノート
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