Hydrochloric Acid → 4(1H)-Pyrimidinone, 3-(2,6-dimethylphenyl)-1-ethyltetrahydro-2-thioxo-

HRID 2393328Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2393328
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][C:10](=[S:19])[N:11]([CH2:14][CH2:15][C:16](O)=[O:17])[CH2:12][CH3:13].Cl>CC(C)=O>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]1[C:16](=[O:17])[CH2:15][CH2:14][N:11]([CH2:12][CH3:13])[C:10]1=[S:19]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 18975625HCID 18975625, Verbindung

Produkt 1

HCID 113115614(1H)-Pyrimidinone, 3-(2,6-dimethylphenyl)-1-ethyltetrahydro-2-thioxo-Ausbeute 47,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

3-[3-(2,6-dimethylphenyl)-1-ethyl-thioureido]propionic acid (12 g) was dissolved in acetone (245 mL). Conc. HCl (5 mL) was added and the mixture was heated at reflux for 18 hours. The reaction mixture was evaporated to dryness. The residue was dissolved in methylene chloride (100 mL), and washed with 1N NaOH. The organic phase was dried over anhydrous magnesium sulfate, then evaporated to dryness. The solid was recrystallized from ethyl acetate to give the title compound (5.3 g) as a white solid, m.p. 124°-126° C.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 18 hours
  3. customThe reaction mixture was evaporated to dryness
  4. dissolutionThe residue was dissolved in methylene chloride (100 mL)
  5. washwashed with 1N NaOH
  6. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  7. customevaporated to dryness
  8. customThe solid was recrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-04600c432d684dc08cc38c7b1c728ebe
Quelldatensatz
uspto-grants-1998_09
Patentnummer
US05807864

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