反応式
[OH:1][C:2]1[C:10]([OH:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH2:17](O)[CH3:18]>>[OH:1][C:2]1[C:10]([OH:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH2:17][CH3:18])=[O:5]参加物
4
実験手順
A mixture of 2,3-dihydroxybenzoic acid(994 g), ethanol (3.8 L) and sulfuric acid (320 g) was refluxed for 44 hours. A portion of the solvent distilled out of the solution, and the solution was cooled and stirred overnight, and then further cooled in an ice/water bath. To the solution was added water (5.6 L). The solution was aged, and the crystals were filtered, washed with water, and dried to give ethyl 2,3-dihydroxybenzoate (1002 g, 85%); m.p. 66.0-67.2° C.
後処理
- temperaturewas refluxed for 44 hours
- distillationA portion of the solvent distilled out of the solution
- temperaturethe solution was cooled
- temperaturefurther cooled in an ice/water bath
- additionTo the solution was added water (5.6 L)
- filtrationthe crystals were filtered
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-532a442dbe104eeaad20cd38b10f718b
- 出典データセット
- uspto-grants-2001_01
- 特許番号
- US06172062B2
関連ノート
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