반응식
[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]참가 물질
실험 절차
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 was 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.
후처리
- extractionthe aqueous solution was 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
출처 및 근거
- ORD 기록
- ord-2ee73a906fa1481c8c8650d9dbd3098f
- 출처 데이터셋
- uspto-grants-1985_06
- 특허 번호
- US04525361
연결된 노트
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