1,2-Dichlorobenzene → 2-Diphenylmethylimino-1,2,3,4,5,6-hexahydro-1,3-dimethylpyrimidine hydroiodide

HRID 46638Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 46638
[IH:1].[C:2]1([CH:8]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[NH:9][C:10](=[NH:13])SC)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:20][NH:21][CH2:22][CH2:23][CH2:24]NC.Cl[C:28]1C=CC=CC=1Cl>>[IH:1].[C:2]1([CH:8]([N:9]=[C:10]2[N:21]([CH3:20])[CH2:22][CH2:23][CH2:24][N:13]2[CH3:28])[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 3

HCID 72391,2-DichlorobenzeneHCID 66978N,N'-Dimethyl-1,3-propanediamineHCID 178504030HCID 178504030, Verbindung

Produkt 1

HCID 202981422-Diphenylmethylimino-1,2,3,4,5,6-hexahydro-1,3-dimethylpyrimidine hydroiodideAusbeute 59,8 %

Versuchsvorschrift

To 38.43 grams (0.10 mole) of 1-diphenylmethyl-2-methyl-2-thiopseudourea hydroiodide in 200 milliliters of o-dichlorobenzene was added 10.22 grams (0.10 mole) of N,N'-dimethyl-1,3-propanediamine and the resulting mixture heated under reflux for 21 hours. The reaction mixture was cooled, the solvent decanted therefrom and isopropanol added to the gummy residue to obtain 24.35 grams (59.8 percent yield) of 2-diphenylmethylimino-1,2,3,4,5,6-hexahydro-1,3-dimethylpyrimidine hydroiodide product of m.p. 215°-219° C. After two recrystallizations from methanol-isopropanol, a purified product, m.p. 221° C., was obtained.

Aufarbeitung

  1. temperaturethe resulting mixture heated
  2. temperatureunder reflux for 21 hours
  3. temperatureThe reaction mixture was cooled
  4. customthe solvent decanted
  5. additionisopropanol added to the gummy residue

Quellen und Nachweise

ORD-Eintrag
ord-4be0b177f4be4a8d89e792821c938622
Quelldatensatz
uspto-grants-1979_11
Patentnummer
US04174401

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