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3-Hydroxybutyric Acid → Dodecyl 3-Hydroxybutyrate

HRID 256799
ノート
印刷プレビュー

反応式

HRID 256799 の反応式
[OH:1][CH:2]([CH3:7])[CH2:3][C:4]([OH:6])=[O:5].[CH2:8](O)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]>S(=O)(=O)(O)O>[CH2:19]([O:5][C:4](=[O:6])[CH2:3][CH:2]([OH:1])[CH3:7])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4413-Hydroxybutyric AcidHCID 81931-Dodecanol

生成物 1

HCID 18955122Dodecyl 3-Hydroxybutyrate収率 62.6%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

実験手順

A 500 ml one neck round bottom flask equipped with a Dean Stark trap, condenser and nitrogen inlet/outlet was charged with 72.0 g (0.69 moles) 3- hydroxybutyric acid, 268.5 g (1.45 moles) dodecyl alcohol, and 0.36 g sulfuric acid (based on 0.5 g/mole 3-hydroxybutyric acid). The mixture was heated to 115 degrees for 48 hours and water was collected as the reaction proceeded. The acid was neutralized by washing three times with 100 ml saturated sodium bicarbonate solution. The organic layer was collected and dried over magnesium sulfate. Excess dodecyl alcohol was removed by high vacuum distillation to yield 117.65 g (60% yield) of clear oil (91% pure by GC).

後処理

  1. temperatureThe mixture was heated to 115 degrees for 48 hours
  2. customwater was collected as the reaction
  3. washby washing three times with 100 ml saturated sodium bicarbonate solution
  4. customThe organic layer was collected
  5. dry with materialdried over magnesium sulfate
  6. customExcess dodecyl alcohol was removed by high vacuum distillation

出典と根拠

ORDレコード
ord-a47b2d80e9cc48ca9fbd823d760c630e
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05260051

反応ノート

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