2,6-Dihydroxybenzoic Acid → 2,6-Diacetoxybenzoic acid
反応式
[OH:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([OH:11])[C:3]=1[C:4]([OH:6])=[O:5]>CC(OC(C)=O)=O.OS(O)(=O)=O>[C:2]([O:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][C:7](=[O:11])[CH3:8])[C:3]=1[C:4]([OH:6])=[O:5])(=[O:1])[CH3:3]参加物
4
実験手順
A solution of 2,6-dihydroxybenzoic acid (4.72 g, 30 mmol) in Ac2O (16 g, 14.2 mL) containing 5 drops of conc. H2SO4 was heated with stirring at 80° for 2 hr until tlc analysis indicated the reaction was complete. The solution was poured onto ice/H2O and extracted 3× with EtOAc. The combined organic phases were washed 4× with H2O and once with brine prior to drying over Na2SO4. After removal of the volatiles using a rotary evaporator, 5.8 g of 2,6-diacetoxybenzoic acid was obtained as a white solid which was used without further purification.
後処理
- temperaturewas heated
- additionThe solution was poured onto ice/H2O
- extractionextracted 3× with EtOAc
- washThe combined organic phases were washed 4× with H2O
- dry with materialonce with brine prior to drying over Na2SO4
- customAfter removal of the volatiles
- customa rotary evaporator
出典と根拠
- ORDレコード
- ord-10a7ef1656d4431e99bfd2cc237a2e72
- 出典データセット
- uspto-grants-2003_04
- 特許番号
- US06555519B2
反応ノート
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