Acetone → HCID 20382884, Verbindung

HRID 1415578Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1415578
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:17]=[CH:16][C:9]([C:10]([NH:12][CH2:13][CH2:14][OH:15])=[O:11])=[CH:8][CH:7]=1)=[O:4].[S:18]1C=CC=C1CC([O-])=O.[K+].[CH3:28][C:29](C)=[O:30]>>[C:29]([S:18][CH2:2][C:3]([NH:5][C:6]1[CH:17]=[CH:16][C:9]([C:10]([NH:12][CH2:13][CH2:14][OH:15])=[O:11])=[CH:8][CH:7]=1)=[O:4])(=[O:30])[CH3:28]

Komponenten

4

Edukt 3

HCID 180AcetoneHCID 203829064-(2-Chloroacetamido)-N-(2-hydroxyethyl)benzamideHCID 23696799Potassium 2-thienylacetate

Produkt 1

HCID 20382884HCID 20382884, VerbindungAusbeute 57 %

Versuchsvorschrift

-- A mixture of 4-(2-chloroacetamido)-N-(2-hydroxyethyl)benzamide (39.3 g., 0.153 mole) and potassium thiolacetate (18.3 g., 0.16 mole) in 650 ml. of acetone is heated at reflux temperature for a period of 2 hr. After standing overnight, the reaction mixture is filtered, the filtercake washed with acetone, slurried with water, filtered and the filtercake washed with water and dried to afford 34.7 g. of crude product. Crystallization of this material from ethyl acetate-methanol affords analytically pure 4-[2-(ACETYLTHIO)ACETAMIDO]-N-(2-HYDROXYETHYL)BENZAMIDE, m.p. 190.0°-192.0° C. (corr.) in 57% yield.

Aufarbeitung

  1. temperatureat reflux temperature for a period of 2 hr
  2. filtrationthe reaction mixture is filtered
  3. washthe filtercake washed with acetone
  4. filtrationfiltered
  5. washthe filtercake washed with water
  6. customdried
  7. customto afford 34.7 g
  8. customCrystallization of this material from ethyl acetate-methanol

Quellen und Nachweise

ORD-Eintrag
ord-39088294726947cdafdba90fffc30946
Quelldatensatz
uspto-grants-1977_01
Patentnummer
US04005222

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