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Lactic Acid → 2-Propynyl 2-hydroxypropionate

HRID 2275980
ノート
印刷プレビュー

反応式

HRID 2275980 の反応式
[OH:1][CH:2]([CH3:6])[C:3]([OH:5])=[O:4].[CH2:7](O)[C:8]#[CH:9].S(=O)(=O)(O)O.C([O-])(=O)C.[Na+]>C1(C)C=CC=CC=1>[OH:1][CH:2]([CH3:6])[C:3]([O:5][CH2:9][C:8]#[CH:7])=[O:4]
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 4

HCID 612Lactic AcidHCID 1118Sulfuric AcidHCID 7859Propargyl alcoholHCID 517045Sodium Acetate

生成物 1

HCID 866519122-Propynyl 2-hydroxypropionate収率 45%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

52.99 g (0.50 mol) of an aqueous solution of 85% 2-hydroxypropionic acid and 45 mL of toluene were dissolved in 84.09 g (1.50 mol) of propargyl alcohol, and 1.0 mL of concentrated sulfuric acid was added thereto. Using a Dean-Stark device under normal pressure, the formed water was removed from the system, and this was further reacted under reflux under normal pressure. After 3 hours, the reaction liquid was analyzed through liquid chromatography, and the disappearance of the starting materials was confirmed. Then, the reaction liquid was neutralized with sodium acetate added thereto, filtered, and the filtrate was concentrated. The residue was purified through reduced pressure distillation to give 28.81 g (45% yield) of 2-propynyl 2-hydroxypropionate.

後処理

  1. customthe formed water was removed from the system
  2. customthis was further reacted
  3. temperatureunder reflux under normal pressure
  4. customthe reaction liquid
  5. customThen, the reaction liquid
  6. additionadded
  7. filtrationfiltered
  8. concentrationthe filtrate was concentrated
  9. distillationThe residue was purified through reduced pressure distillation

出典と根拠

ORDレコード
ord-c9cc4ff08c464414ae357555e93d2f90
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09130244B2

反応ノート

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