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Thioglycolic Acid → HCID 20348735, Verbindung

HRID 1701155
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1701155
[SH:1][CH2:2][C:3]([OH:5])=[O:4].[OH-].[K+].[F:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[CH:20]=[CH:19][C:18]([CH:21](Cl)[CH3:22])=[CH:17][CH:16]=1.C1(C)C=CC=CC=1>CO.O>[F:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[CH:16]=[CH:17][C:18]([CH:21]([S:1][CH2:2][C:3]([OH:5])=[O:4])[CH3:22])=[CH:19][CH:20]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 1133Thioglycolic AcidHCID 1140TolueneHCID 14797Potassium HydroxideHCID 203487834'-(1-Chloroethyl)-2-fluoro-1,1'-biphenyl

Produkt 1

HCID 20348735HCID 20348735, VerbindungAusbeute 55 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887
Methanol
Lösungsmittel
HCID 962WaterLösungsmittel2×

Versuchsvorschrift

6.35 gm (0.055 mol) of 80% mercaptoacetic acid were admixed in 70 ml of methanol with a solution of 6.2 gm (0.11 mol) of potassium hydroxide in 6.2 ml of water. To the solution of dipotassium salt, 11.7 gm (0.05 mol) of 1-(2'-fluoro-4-biphenylyl)-1-chloro-ethane were added, the reaction mixture was rinsed with 20 ml of methanol and stirred for 18 hours at room temperature. Subsequently, the mixture was evaporated, the residue was digested with acetone, and the precipitated potassium salt was suction-filtered off. The free acid was obtained by dissolving the salt in water and acidifying the solution. M.p 128°-130° C. (from toluene). Yield: 55% of theory.

Aufarbeitung

  1. washthe reaction mixture was rinsed with 20 ml of methanol
  2. customSubsequently, the mixture was evaporated
  3. filtrationthe precipitated potassium salt was suction-filtered off
  4. customThe free acid was obtained

Quellen und Nachweise

ORD-Eintrag
ord-84eb262934c24fdab5d2cb07f93fb5d2
Quelldatensatz
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04191776

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