Tetrahydrofuran → HCID 15725166、化合物

HRID 1085679ノート

反応式

HRID 1085679 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].O1CCCC1.[CH3:12][C:13]1[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][C:14]=1[O:15][CH:16]([CH3:20])[C:17](O)=[O:18].[OH-].[Na+]>O>[CH3:12][C:13]1[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][C:14]=1[O:15][CH:16]([CH3:20])[CH2:17][OH:18]

参加物

6

反応物 4

HCID 8028Tetrahydrofuran2 回HCID 14798Sodium HydroxideHCID 42078482-(2,5-dimethylphenoxy)propanoic acidHCID 21226445Aluminium lithium hydride

生成物 1

HCID 15725166HCID 15725166、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a stirred and refluxing mixture of 56 parts of lithium aluminum hydride in 1000 parts of tetrahydrofuran was added dropwise a solution of 359 parts of 2-(2,5-dimethylphenoxy)propanoic acid in 1000 parts of tetrahydrofuran. Upon completion, stirring was continued at reflux temperature for 1.50 hours. The reaction mixture was cooled and decomposed by the successive additions of 55 parts of water, 45 parts of a 15% sodium hydroxide solution and 190 parts of water and the whole was stirred for 30 minutes. The inorganic material was filtered off after acidification with hydrochloric acid solution. The filtrate was dried, filtered and evaporated. The residue was distilled, yielding 73 parts of 2-(2,5-dimethylphenoxy)-1-propanol; bp. 150° C. at 11 mm. pressure (131).

後処理

  1. temperaturerefluxing
  2. stirringUpon completion, stirring
  3. temperatureat reflux temperature for 1.50 hours
  4. temperatureThe reaction mixture was cooled
  5. stirringthe whole was stirred for 30 minutes
  6. filtrationThe inorganic material was filtered off after acidification with hydrochloric acid solution
  7. customThe filtrate was dried
  8. filtrationfiltered
  9. customevaporated
  10. distillationThe residue was distilled

出典と根拠

ORDレコード
ord-eb72ea6ada0d49538bab83e450e167c6
出典データセット
uspto-grants-1991_04
特許番号
US05010198

反応ノート

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