Acetic Anhydride → 4-Methoxy-1,3-dihydro-2-benzofuran-1,3-dione

HRID 425219

反応式

HRID 425219 の反応式
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

反応物 2

HCID 7918Acetic AnhydrideHCID 3152183-Methoxyphthalic acid

生成物 1

HCID 2911934-Methoxy-1,3-dihydro-2-benzofuran-1,3-dione収率 99.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

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

  1. temperatureat reflux for 4 hours
  2. customwas removed in vacuo
  3. 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-8a819cea0854430cb06c5d27910cdb4f
出典データセット
uspto-grants-2012_01
特許番号
US08106057B2

関連ノート

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