Acetyl chloride → 7-Methoxyisochroman-1,3-dione
반응식
[C:1]([CH2:4][C:5]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][C:6]=1[C:7]([OH:9])=[O:8])(O)=[O:2].C(Cl)(=O)C>CC(C)=O>[CH3:15][O:14][C:11]1[CH:10]=[C:6]2[C:5]([CH2:4][C:1](=[O:2])[O:8][C:7]2=[O:9])=[CH:13][CH:12]=1참가 물질
4
실험 절차
To a suspension of 2-(carboxymethyl)-5-methoxybenzoic acid (5.22 g) (synthesised using the procedure in Tetrahedron 1975, 31, 2607-19) in acetone (50 ml) was added acetyl chloride (7.06 ml) and the reaction mixture was stirred at room temperature for 18 hours. The solvent was evaporated and azeotroped with toluene (×3). The resultant solid was triturated with diethyl ether to yield 7-methoxy-1H-isochromene-1,3(4H)-dione as a brown solid (4.36 g); NMR Spectrum: (DMSOd6) 3.84 (s, 3H), 4.20 (s, 2H), 7.36 (m, 2H), 7.50 (s, 1H).
후처리
- customsynthesised
- customThe solvent was evaporated
- customazeotroped with toluene (×3)
- customThe resultant solid was triturated with diethyl ether
출처 및 근거
- ORD 기록
- ord-b03248ada40044e7a266c5a37c696810
- 출처 데이터셋
- uspto-grants-2010_08
- 특허 번호
- US07786115B2
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