反応式
[OH-:1].[Na+:2].[C:3]1([C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6][O:5]1)=[O:4]>>[OH:1][CH2:6][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:12]=1[C:3]([O-:5])=[O:4].[Na+:2]参加物
3
実験手順
An aqueous solution (200 ml) of phthalide (134 g) and sodium hydroxide (40 g) was heated. After stirring for 1 hour, the mixture was concentrated under reduced pressure for removal of water to obtain sodium 2-hydroxymethylbenzoate as colorless crystals. p-Cymene (480 ml) and 2,5-xylenol (122 g) were added to the crystals. Azeotropic dehydration was carried out with heating under reflux for 7 hours by using an azeotropic dehydration apparatus. After cooling, ice water was added. Concentrated hydrochloric acid was added dropwise to make the mixture acidic. The precipitates were separated by filtration and recrystallized from ethyl acetate to obtain the title compound (155 g, Yield: 60.5%), mp: 162°-163° C.
後処理
- concentrationthe mixture was concentrated under reduced pressure for removal of water
出典と根拠
- ORDレコード
- ord-983c05e8d50d4792ab1663b81eb89440
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05414122
関連ノート
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