反応式
[CH3:1][O:2][C:3]1[C:4](=[O:24])[C:5]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][OH:23])=[C:6]([CH3:12])[C:7](=[O:11])[C:8]=1[O:9][CH3:10].[C:25](OC(=O)C)(=[O:27])[CH3:26]>N1C=CC=CC=1.O>[CH3:1][O:2][C:3]1[C:4](=[O:24])[C:5]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][O:23][C:25](=[O:27])[CH3:26])=[C:6]([CH3:12])[C:7](=[O:11])[C:8]=1[O:9][CH3:10]参加物
実験手順
To a cooled, well stirred solution of 2,3-dimethoxy-5-methyl-6-(10'-hydroxydecyl)-1,4-benzoquinone (formula IV-2 wherein R=H3CO, n=8, in the free form) (0.3 part) in pyridine (1 volume part) was added acetic anhydride (0.1 volume part). After stirring at room temperature for 1 hour, the mixture was diluted with water, and the aqueous solution as extracted with diethyl ether. The extract was washed successively with water, dilute hydrochloric acid, water, saturated aqueous sodium hydrogen carbonate and water, and dried over anhydrous sodium sulfate. The residue upon removal of the solvent was crystallized from aqueous ethanol to give 2,3-dimethoxy-5-methyl-6-(10'-acetoxydecyl)-1,4-benzoquinone (formula IV-2 wherein R=H3CO, n=8, in the form of acetate) (0.31 part) as orange needles melting at 38° C.
後処理
- extractionthe aqueous solution as extracted with diethyl ether
- washThe extract was washed successively with water, dilute hydrochloric acid, water, saturated aqueous sodium hydrogen carbonate and water
- dry with materialdried over anhydrous sodium sulfate
- customThe residue upon removal of the solvent
- customwas crystallized from aqueous ethanol
出典と根拠
- ORDレコード
- ord-05ff427503a94a39857951bdada6eeed
- 出典データセット
- uspto-grants-1983_10
- 特許番号
- US04407757
関連ノート
読み込み中…