Acetic Anhydride → 4-Methoxy-1,3-dihydro-2-benzofuran-1,3-dione
反応式
C(OC(=O)C)(=O)C.[CH3:8][O:9][C:10]1[CH:18]=[CH:17][CH:16]=[C:12]([C:13]([OH:15])=O)[C:11]=1[C:19]([OH:21])=[O:20]>O1CCCC1>[CH3:8][O:9][C:10]1[CH:18]=[CH:17][CH:16]=[C:12]2[C:13]([O:21][C:19](=[O:20])[C:11]=12)=[O:15]参加物
4
実験手順
Acetic anhydride (70 ml) was added to a mixture of 3-methoxyphthalic acid (51.0 g, 0.26 mol) in anhydrous tetrahydrofuran (250 ml) and the mixture was stirred and held at reflux for 4 hours. Upon cooling to room temperature the solvent was removed in vacuo and the resulting solid material was dried in a vacuum oven at 50° C. overnight to afford 3-methoxyphthalic anhydride (45.9 g, 99%) as a colourless solid. 1H NMR (DMSO-d6) 7.97 (1H, dd), 7.63 (1H, d), 7.60 (1H, d), 4.02 (3H, s). MS: [M+H]+ 179.
後処理
- temperatureat reflux for 4 hours
- customwas removed in vacuo
- customthe resulting solid material was dried in a vacuum oven at 50° C. overnight
出典と根拠
- ORDレコード
- ord-b87ec722220d4e5a9b025b8776c4a2a7
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08530469B2
反応ノート
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