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Water → 2-(3-Hydroxypropyl)-2-phenyl-1,3-dioxolane

HRID 1601327
ノート
印刷プレビュー

反応式

HRID 1601327 の反応式
C1[O:17][C:4](OC)([CH2:5][CH2:6][C:7](=[O:14])[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)OC1.[H-].[H-].[H-].[H-].[Li+].[Al+3].O.[OH-].[K+].C1C[O:30][CH2:29][CH2:28]1>>[CH2:28]1[O:14][C:7]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)([CH2:6][CH2:5][CH2:4][OH:17])[O:30][CH2:29]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 962Water2 回HCID 8028Tetrahydrofuran2 回HCID 14797Potassium HydroxideHCID 21226445Aluminium lithium hydrideHCID 86754745Methyl 3-benzoylpropionate ethylene ketal

生成物 1

HCID 223445572-(3-Hydroxypropyl)-2-phenyl-1,3-dioxolane収率 93%

実験手順

A solution of methyl 3-benzoylpropionate ethylene ketal (7.9661 g, 33.7 mmol), prepared in the previous step in 150 ml of anhydrous THF was added under nitrogen dropwise over 1 hour to a suspension of LAH (1.6656 g, 43.9 mmol) in 75 ml of anhydrous THF. After the addition the mixture was stirred at room temperature for 19 hours. Water (1.7 ml) was then added dropwise followed by the addition of 1.7 ml of 15% KOH and then 5.1 ml of water. The resulting mixture was stirred for 15 minutes and then filtered. The filtrate was concentrated under reduced pressure to remove most of the THF. The residue was partitioned between methylene chloride-water. The organic layer was separated and the aqueous layer extracted two times with methylene chloride. The combined organic extracts were dried (MgSO4) and the solvent removed under reduced pressure to give 4-hydroxybutyrophenone ethylene ketal (6.51 g, 93%) as a white solid, mp 39-42° C.

後処理

  1. additionAfter the addition the mixture
  2. stirringThe resulting mixture was stirred for 15 minutes
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customto remove most of the THF
  6. customThe residue was partitioned between methylene chloride-water
  7. customThe organic layer was separated
  8. extractionthe aqueous layer extracted two times with methylene chloride
  9. dry with materialThe combined organic extracts were dried (MgSO4)
  10. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-555d9f70bd00448eb8871e62124a2aa0
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05977170

反応ノート

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