Valproic Acid → 4-Hydroxybutyl 2-propylpentanoate

HRID 41817

反応式

HRID 41817 の反応式
[CH2:1]([CH:4]([CH2:8][CH2:9][CH3:10])[C:5]([OH:7])=[O:6])[CH2:2][CH3:3].[CH2:11](O)[CH2:12][CH2:13][CH2:14][OH:15]>CS(O)(=O)=O.C1(C)C=CC=CC=1>[CH2:1]([CH:4]([CH2:8][CH2:9][CH3:10])[C:5]([O:7][CH2:11][CH2:12][CH2:13][CH2:14][OH:15])=[O:6])[CH2:2][CH3:3]

参加物

5

反応物 2

HCID 3121Valproic AcidHCID 80641,4-Butanediol

生成物 1

HCID 584553024-Hydroxybutyl 2-propylpentanoate収率 99%

試薬・触媒・溶媒 2

HCID 6395Methanesulfonic Acid触媒HCID 1140Toluene溶媒

実験手順

2-propylpentanoic acid (40.16 g, 278.5 mmol) was mixed with butane-1-4-diol (114.65 g, 1272.2 mmol) and methyl-sulfonic acid (5 drops) in toluene (3500 ml) and the mixture was heated under reflux using a Dean Stark trap for 12 h. After that, toluene was removed under reduced pressure and the crude mixture was dissolved in chloroform (200 ml) and extracted with water (pH 5, 3×200 ml). The combined organic layers were dried over sodium sulfate and the volatiles were removed under reduced pressure giving a clear oil (99%).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. customfor 12 h
  4. customAfter that, toluene was removed under reduced pressure
  5. dissolutionthe crude mixture was dissolved in chloroform (200 ml)
  6. extractionextracted with water (pH 5, 3×200 ml)
  7. dry with materialThe combined organic layers were dried over sodium sulfate
  8. customthe volatiles were removed under reduced pressure

出典と根拠

ORDレコード
ord-bfee8a1339084b148a77c82b91b7385d
出典データセット
uspto-grants-2013_09
特許番号
US08535655B2

関連ノート

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