Water → 2-[2-(Hydroxymethyl)phenyl]ethanol

HRID 2706

反応式

HRID 2706 の反応式
[C:1](O)(=[O:12])[CH2:2][C:3]1[C:4](=[CH:8][CH:9]=[CH:10][CH:11]=1)[C:5](O)=[O:6].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[OH:6][CH2:5][C:4]1[CH:8]=[CH:9][CH:10]=[CH:11][C:3]=1[CH2:2][CH2:1][OH:12]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 66643Homophthalic acidHCID 21226445Aluminium lithium hydride

生成物 1

HCID 2390242-[2-(Hydroxymethyl)phenyl]ethanol収率 98,293.703%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Dissolve homophthalic acid (22.2 g, 0.123 mmol) in tetrahydrofuran (250 mL) and add dropwise at room temperature to a slurry of lithium aluminum hydride (15.5 g, 0.407 mol) in tetrahydrofuran (500 mL). Heat at reflux for 18 hours, cool in an ice bath and carefully add, by dropwise addition, water (16 mL), followed by 50% sodium hydroxide (16 mL). Remove the ice bath, add water slowly with stirring and stir until the gray precipitate turns white and evolution of gas ceases. Filter, wash solids with methylene chloride, dry (MgSO4) and evaporate the solvent in vacuo to give 2-(2-hydroxymethyl-phenyl)-ethanol as a viscous oil (18.4 g, 98%).

後処理

  1. temperatureHeat
  2. temperatureat reflux for 18 hours
  3. temperaturecool in an ice bath
  4. customRemove the ice bath
  5. additionadd water slowly
  6. stirringstir until the gray precipitate
  7. filtrationFilter
  8. washwash solids with methylene chloride
  9. dry with materialdry (MgSO4)
  10. customevaporate the solvent in vacuo

出典と根拠

ORDレコード
ord-eb64b8ce0a9f4ad097d9d9c05791fc8a
出典データセット
uspto-grants-1998_03
特許番号
US05731306

関連ノート

読み込み中…