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Ethanol → ethyl 3,3,3-trifluoro-2-hydroxypropanoate

HRID 2414920
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2414920
[F:1][C:2]([F:9])([F:8])[CH:3]([OH:7])[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH2:15](O)[CH3:16]>>[F:1][C:2]([F:9])([F:8])[CH:3]([OH:7])[C:4]([O:6][CH2:15][CH3:16])=[O:5]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 2448963,3,3-Trifluoro-2-hydroxypropanoic acid

Produkt 1

HCID 2758935ethyl 3,3,3-trifluoro-2-hydroxypropanoateAusbeute 68 %

Versuchsvorschrift

The step (b) of the present invention was conducted as follows. At first, 2.84 g of the crude product obtained by Example 1 (containing 16.07 mmol (1.00 eq.) of 3,3,3-trifluoro-2-hydroxypropionic acid) and 19.6 mg (0.20 mmol, 0.01 eq.) of 98% sulfuric acid were added to 20 ml of ethanol, followed by stirring for 43 hr with heating under reflux. The resulting reaction liquid itself was subjected to a vacuum distillation (52° C./3,500 Pa), thereby obtaining 1.87 g of white, needle-like crystals of ethyl 3,3,3-trifluoro-2-hydroxypropionate of the following formula 8. The yield was 68%. The obtained crude product (the white, needle-like crystals) was used in the following step (c) of Example 3 without conducting a further purification.

Aufarbeitung

  1. temperaturewith heating
  2. temperatureunder reflux
  3. customThe resulting reaction liquid itself
  4. distillationwas subjected to a vacuum distillation (52° C./3,500 Pa)

Quellen und Nachweise

ORD-Eintrag
ord-1cf44ed070064de390d36da643351433
Quelldatensatz
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06815559B2

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