Potassium Carbonate → 2-(3-Chloro-2-methylph-enyl-thiomethyl)-2-imidazoline hydrochloride

HRID 653657

Reaktionsgleichung

Reaktionsgleichung von HRID 653657
[Cl:1][C:2]1[C:3]([CH3:9])=[C:4]([SH:8])[CH:5]=[CH:6][CH:7]=1.Cl.Cl[CH2:12][C:13]1[NH:14][CH2:15][CH2:16][N:17]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[ClH:1].[Cl:1][C:2]1[C:3]([CH3:9])=[C:4]([S:8][CH2:12][C:13]2[NH:17][CH2:16][CH2:15][N:14]=2)[CH:5]=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 27609282-(chloromethyl)-4,5-dihydro-1H-imidazole hydrochlorideHCID 148782363-Chloro-2-methylbenzenethiol

Produkt 1

HCID 148782382-(3-Chloro-2-methylph-enyl-thiomethyl)-2-imidazoline hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

5.55 g (35 mmol) of 3-chloro-2-methyl-thiophenol, 5.43 g (35 mmol) of 2-chloromethyl-2-imidazoline hydrochloride and 5 g of potassium carbonate are stirred in 40 ml of ethanol at room temperature. After 25 h, the mixture is filtered and the filtrate is concentrated to dryness. The crude product is purified by column chromatography on silica gel. After the eluting agent has been stripped off, ethanolic hydrochloric acid is added to the residue and the product is precipitated by addition of ether. White crystals of melting point 208°-209° C. are obtained.

Aufarbeitung

  1. filtrationthe mixture is filtered
  2. concentrationthe filtrate is concentrated to dryness
  3. customThe crude product is purified by column chromatography on silica gel
  4. additionethanolic hydrochloric acid is added to the residue
  5. customthe product is precipitated by addition of ether
  6. customWhite crystals of melting point 208°-209° C. are obtained

Quellen und Nachweise

ORD-Eintrag
ord-8929725e1b2f4869a090178749328139
Quelldatensatz
uspto-grants-1992_07
Patentnummer
US05128361

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