Water → 1,2-Benzenedimethanol

HRID 472991

反応式

HRID 472991 の反応式
[C:1](O)(=[O:11])[C:2]1[C:3](=[CH:7][CH:8]=[CH:9][CH:10]=1)[C:4](O)=[O:5].[H-].[H-].[H-].[H-].[Li+].[Al+3].O.[OH-].[Na+]>C1COCC1>[C:2]1([CH2:1][OH:11])[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[CH2:4][OH:5]

参加物

6

反応物 4

HCID 962WaterHCID 1017Phthalic AcidHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydride

生成物 1

HCID 691531,2-Benzenedimethanol収率 101.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of phthalic acid (9 g, 0.05 mol) in anhydrous THF (200 mL) was added to LAH (7.6 g, 0.2 mol) in THF (250 mL) dropwise, and the mixture was refluxed for 18 hours. The mixture was cooled in ice bath and carefully added water dropwise, followed by 50% NaOH (150 mL), and then removed the ice bath added water slowly with stirring until the gray precipitate turns white. The mixture was filtrated and the filtrate was concentrated to give crude 1,2-phenylenedimethanol (7 g, 92%).

後処理

  1. temperaturethe mixture was refluxed for 18 hours
  2. temperatureThe mixture was cooled in ice bath
  3. customremoved the ice bath
  4. additionadded water slowly
  5. filtrationThe mixture was filtrated
  6. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-0b8e32ae7fa243aebe9cca9c6f902b45
出典データセット
uspto-grants-2014_01
特許番号
US08633212B2

関連ノート

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