Potassium Carbonate → HCID 178485057, Verbindung

HRID 65755

Reaktionsgleichung

Reaktionsgleichung von HRID 65755
C(=O)([O-])[O-].[K+].[K+].[CH3:7][N:8]([CH2:10][C:11]1[O:15][C:14]([CH2:16][S:17][CH2:18][CH2:19][NH2:20])=[CH:13][CH:12]=1)[CH3:9].CS[C:23](=[N:27][CH3:28])[NH:24][C:25]#[N:26]>C(#N)C.[N+]([O-])([O-])=O.[Ag+]>[C:25]([N:24]=[C:23]([NH:27][CH3:28])[NH:20][CH2:19][CH2:18][S:17][CH2:16][C:14]1[O:15][C:11]([CH2:10][N:8]([CH3:7])[CH3:9])=[CH:12][CH:13]=1)#[N:26]

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 1111031-Cyano-2,3-dimethylisothioureaHCID 1622035-(((2-Aminoethyl)thio)methyl)-N,N-dimethyl-2-furanmethanamine

Produkt 1

HCID 178485057HCID 178485057, VerbindungAusbeute 2,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24470Silver NitrateKatalysatorHCID 6342AcetonitrileLösungsmittel2×

Versuchsvorschrift

To a stirred suspension of potassium carbonate (20.7 g) in a solution of 2-[[[5-(dimethylamino)methyl-2-furanyl]methyl]thio]ethanamine (10.7 g) and N-cyano-N'-methylcarbamimidothioic acid methyl ester (7.1 g) in acetonitrile (107 ml) at 70° was added a solution of silver nitrate (9.35 g) in acetonitrile (20 ml) during 1 hr. The mixture was stirred for 16 hr, the solid filtered and the filtrate evaporated to dryness. The residue was dissolved in ethyl acetate (250 ml). A portion of this (10.5 ml) was washed with water (6 ml), the ethyl acetate layer evaporated to give a solid which was crystallised from isopropylacetate (1.75 ml) giving N"-cyano-N-[2-[[[5-(dimethylaminomethyl)-2-furanyl]methyl]thio]ethyl]-N'-methylguanidine (0.35 g) m.p. 79°-81.5°.

Aufarbeitung

  1. filtrationthe solid filtered
  2. customthe filtrate evaporated to dryness
  3. dissolutionThe residue was dissolved in ethyl acetate (250 ml)
  4. washA portion of this (10.5 ml) was washed with water (6 ml)
  5. customthe ethyl acetate layer evaporated
  6. customto give a solid which
  7. customwas crystallised from isopropylacetate (1.75 ml)

Quellen und Nachweise

ORD-Eintrag
ord-318790c9e4144574998bd1b56b0ef298
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04128658

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