Phenyl Isothiocyanate → HCID 54237642, Verbindung

HRID 647584Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 647584
C[O-].[Na+].I.[NH:5]=[C:6]1[N:10]([CH3:11])[CH:9]=[CH:8][S:7]1.[C:12]1([N:18]=[C:19]=[S:20])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C(O)C.C1(C)C=CC=CC=1>[CH3:11][N:10]1[CH:9]=[CH:8][S:7][C:6]1=[N:5][C:19]([NH:18][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[S:20]

Komponenten

6

Edukt 3

HCID 7673Phenyl IsothiocyanateHCID 10942334Sodium MethoxideHCID 429153603-METHYL-1,3-THIAZOL-2(3H)-IMINE HYDROIODIDE

Produkt 1

HCID 54237642HCID 54237642, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 1140TolueneLösungsmittel

Versuchsvorschrift

Sodium methoxide (5.40 g) was added to a stirred mixture of 2-imino-3-methylthiazoline hydroiodide (24.95 g) in ethanol (100 ml) and the mixture brought to reflux. Phenyl isothiocyanate (16.35 g) in toluene (50 ml) was added over 30 minutes and reflux continued for a further hour then cooled in ice. The solid obtained on filtration and washing with ethanol and water was dried to give the product, mpt 172.5°-173.5°. Recrystallisation from iso-propanol gave analytically pure product, mpt 173.5°-174°.

Aufarbeitung

  1. temperatureto reflux
  2. temperaturereflux
  3. waitcontinued for a further hour
  4. temperaturethen cooled in ice
  5. customThe solid obtained on filtration
  6. washwashing with ethanol and water
  7. customwas dried
  8. customto give the product, mpt 172.5°-173.5°
  9. customRecrystallisation from iso-propanol
  10. customgave analytically pure product, mpt 173.5°-174°

Quellen und Nachweise

ORD-Eintrag
ord-2dd75946f83a4ef09305d7039efdd6e7
Quelldatensatz
uspto-grants-1983_10
Patentnummer
US04409216

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